CN102923754A - Rare earth elements contained laminated dihydroxy composite metal oxide, and preparation method and application thereof - Google Patents
Rare earth elements contained laminated dihydroxy composite metal oxide, and preparation method and application thereof Download PDFInfo
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- CN102923754A CN102923754A CN2011102305369A CN201110230536A CN102923754A CN 102923754 A CN102923754 A CN 102923754A CN 2011102305369 A CN2011102305369 A CN 2011102305369A CN 201110230536 A CN201110230536 A CN 201110230536A CN 102923754 A CN102923754 A CN 102923754A
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Abstract
The invention relates to a rare earth elements contained laminated dihydroxy composite metal oxide, and a preparation method and an application thereof. The rare earth elements contained laminated dihydroxy composite metal oxide is synthesized through treating a salt containing metal elements comprising La, Cu, Mg and Fe as a raw material, and is used for adsorbing and removing As in water. The preparation method comprises the following technological steps: preparing a solution 1 containing certain concentrations of La, Cu, Mg and Fe, and preparing a solution 2 containing certain concentrations of sodium hydroxide and sodium carbonate; adding the solution 1 and the solution 2 into a beaker containing a certain amount of deionized water at certain speeds in a dropwise manner while stirring; and ageing a solution obtained after a reaction and containing a precipitate at a certain temperature for a period of time, centrifuging, repeatedly flushing the precipitate with deionized water until the supernatant is neutral, and drying to obtain the rare earth element contained laminated dihydroxy composite metal oxide which is an adsorbent product. Compared with products in the prior art, the product provided by the invention can realize the effective treatment and purification of the water polluted by As, and has the advantages of high utilization rate, low cost and the like.
Description
Technical field
The invention belongs to the processing technology field of arsenic and heavy metal contamination in the water, relate to and utilize synthetic copper, magnesium, the iron of containing of chemical reagent, contain simultaneously the layered di-hydroxyl composite metal oxidate of rare earth element as sorbent material, and be applied to the removal of arsenic and heavy metal ion in the water, realize contaminated water purification.
Background technology
Arsenic contamination is global problem to the harm of HUMAN HEALTH, has in the world tens countries that the arsenic contamination event in large zone occurs at present.China is that this respect pollutes one of comparatively serious country, and arsenic contamination affects the ground urban residents' such as NORTHWEST CHINA area drinking water safety always.At present, the removal method of arsenic in water body comprised coagulation, co-precipitation, membrane sepn, absorption etc.Absorption method is used widely in the tap water engineering with its economical and efficient, the advantage such as easy to operate.
Layered di-hydroxyl composite metal oxidate (LDHs) is to assemble the compound that forms by positively charged main body laminate and interlayer anion by the interaction of non covalent bond.Traditional LDHs is that the aluminum ion by the magnesium ion of divalence and trivalent consists of, and the LDHs material that contains copper, magnesium, iron ion when also not containing rare earth element so far is used for the correlative study report that arsenic in water body is removed.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of technique simple in order to overcome the defective that above-mentioned prior art exists, and the absorption property of product is good contains layered di-hydroxyl composite metal oxidate of rare earth element and its preparation method and application.
Purpose of the present invention can be achieved through the following technical solutions: a kind of layered di-hydroxyl composite metal oxidate that contains rare earth element, it is characterized in that this oxide compound is to contain the simultaneously layered di-hydroxyl composite metal oxidate of cupric, magnesium, three kinds of elements of iron of rare earth element.
A kind of preparation method who contains the layered di-hydroxyl composite metal oxidate of rare earth element is characterized in that the method may further comprise the steps:
(1) preparation of solution
The salt of Cu, Mg, Fe and rare earth element is dissolved in the deionized water, is mixed with solution 1, contain Cu in the solution 1
2+, Mg
2+, Fe
3+Be respectively 20mmolL with the concentration of rare earth element
-1～500mmolL
-1Get Na
2CO
3Be dissolved in the deionized water with NaOH, be mixed with solution 2, contain Na in the solution 2
2CO
3Be respectively 400mmolL with the concentration of NaOH
-1～2000mmolL
-1
(2) building-up process
Solution 1 and solution 2 are mixed in the adding deionized water mutually, make Cu
2+, Mg
2+, Fe
3+Four metal ion species amount of substance sum and Na with rare earth element
2CO
3With the ratio of NaOH amount of substance sum be (0.1～10): 1, stirring reaction simultaneously, keeping the pH value in the reaction process is 8.5～13.5;
(3) ageing and oven dry
After step (2) reaction is finished, the solution that obtains, the at a certain temperature ageing regular hour is with the solution centrifugal after the ageing, the throw out that separation is obtained is neutral with deionized water rinsing to supernatant liquor repeatedly, and then oven dry obtains product at a certain temperature.
The salt of the described Cu of step (1), Mg, Fe and rare earth element is nitrate, hydrochloride or vitriol, and described rare earth element is La.
The speed of the described stirring reaction of step (2) is 50～1000rpm.
The temperature of the described ageing of step (3) is 15～90 ℃, and the time of ageing is 6h～48h, and bake out temperature is 70 ℃～250 ℃.
A kind of application that contains the layered di-hydroxyl composite metal oxidate of rare earth element, it is characterized in that, taking by weighing the layered di-hydroxyl composite metal oxidate that contains rare earth element joins in the arsenic-containing water solution, after the pH value with acid or alkaline solution regulator solution, place the thermostat container of the certain temperature certain hour that vibrates, then, measure the concentration of arsenic in the supernatant liquor, according to the concentration difference of arsenic in the water before and after the absorption, determine that sorbent material is to the adsorptive capacity of arsenic element in the water.
The concentration range of arsenic is 1～500mg/L in the described arsenic-containing water solution, and the described concentration of layered di-hydroxyl composite metal oxidate in arsenic-containing water solution that contains rare earth element is 0.1-0.3g/L.
The alkali of the pH of described regulator solution is sodium hydroxide or ammoniacal liquor, and acid is hydrochloric acid, nitric acid or sulfuric acid, and the pH scope of solution is 3.0～11.0.
The oscillation rate of described thermostat container is 50～500rpm, and duration of oscillation is 1～48 hour, and the vibration temperature is 15～50 ℃.
Compared with prior art, the present invention has synthesized the layered di-hydroxyl composite metal oxidate that contains rare earth element, in conjunction with the absorption of adsorption technology for water body pollutent arsenic, has realized effective removal of arsenic in the water.Has easy to prepare, utilising efficiency advantages of higher.
Description of drawings
Fig. 1 is the process flow sheet of the inventive method;
Fig. 2 is the application example path profile that the present invention contains arsenic in the hydroxy composite metal oxide material planar water of rare earth element, copper, magnesium, iron simultaneously.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Embodiment 1:
Shown in Fig. 1-2, a kind of preparation method who contains the layered di-hydroxyl composite metal oxidate of rare earth element reaches this layered di-hydroxyl composite metal oxidate that contains rare earth element the Adsorption of arsenic is used, and step is as follows:
(1) solution 1 of configuration 100ml contains Cu in the solution 1
2+, Mg
2+, Fe
3+, La
3+, Cu wherein
2+Concentration be 20mmolL
-1, Mg
2+Concentration be 60mmolL
-1, Fe
3+Concentration be 20mmolL
-1, La
3+Concentration be 20mmolL
-1Other disposes the solution 2 of 100ml, contains Na in the solution 2
2CO
3And NaOH, Na
2CO
3Concentration be 400mmolL
-1, the concentration of NaOH is 400mmolL
-1
(2) the above-mentioned solution that configures 1 and solution 2 are added drop-wise to certain speed in the beaker of the deionized water that contains 100ml, carry out vigorous stirring in the dropping process, stirring velocity is 1000rpm, and the pH value of controlling simultaneously reaction process remains on about 11.
(3) with reacted solution at 15 ℃ of lower ageing 48h, centrifugal, and repeatedly wash throw out with deionized water, reach neutral to the pH value of supernatant liquor.150 ℃ of lower oven dry, with mortar grinds powder.
(4) take by weighing the layered adsorbent of 0.0200g aforesaid method preparation, place 100ml to contain the arsenate solution of 5.0mg/L pentavalent arsenic, take the pH of sodium hydroxide solution and hydrochloric acid soln regulator solution as 6.Solution was placed constant-temperature shaking incubator 24 hours, and oscillation rate is 150rpm, the concentration of arsenic in the solution behind the use ICP measured reaction, and the result shows that this sorbent material reaches 16mg/g to the loading capacity of pentavalent arsenic.
Embodiment 2:
(1) solution 1 of configuration 50ml contains Cu in the solution 1
2+, Mg
2+, Fe
3+And La
3+, Cu wherein
2+Concentration be 500mmolL
-1, Mg
2+Concentration be 500mmolL
-1, Fe
3+Concentration be 500mmolL
-1, La
3+Concentration be 500mmolL
-1Other disposes the solution 2 of 50ml, contains Na in the solution 2
2CO
3And NaOH, Na
2CO
3Concentration be 2000mmolL
-1, the concentration of NaOH is 2000mmolL
-1
(2) the above-mentioned solution that configures 1 and solution 2 are added drop-wise to certain speed in the beaker of the deionized water that contains 200ml, beaker carries out vigorous stirring in the dropping process, and the pH value of controlling simultaneously reaction process remains on about 10.
(3) with reacted solution 35 ℃ of lower ageings, centrifugal, and repeatedly wash with deionized water, reach neutral to the pH value of supernatant liquor.120 ℃ of lower oven dry, with mortar grinds powder.
(4) take by weighing the layered adsorbent of 0.0500g aforesaid method preparation, place 250ml to contain the arsenious arsenite solution of 5.0mg/L, take the pH of sodium hydroxide solution and hydrochloric acid soln regulator solution as 5.5.Solution was placed constant-temperature shaking incubator 12 hours, and oscillation rate is 250rpm, arsenious concentration in the solution behind the use ICP measured reaction, and the result shows that this sorbent material reaches 12mg/g to arsenious loading capacity.
A kind of preparation method who contains the layered di-hydroxyl composite metal oxidate of rare earth element is characterized in that the method may further comprise the steps:
(1) preparation of solution
With Cu (NO
3)
2, Mg (NO
3)
2, Fe (NO
3)
3And La (NO
3)
3Be dissolved in the deionized water, be mixed with solution 1, Cu in the solution 1
2+Concentration be 100mmolL
-1, Mg
2+Concentration be 20mmolL
-1, Fe
3+Concentration be 30mmolL
-1, La
3+Concentration be 30mmolL
-1Get Na
2CO
3Be dissolved in the deionized water with NaOH, be mixed with solution 2, contain Na in the solution 2
2CO
3Be 800mmolL with the concentration of NaOH
-1
(2) building-up process
Solution 1 and solution 2 are mixed in the deionized water mutually, make Cu
2+, Mg
2+, Fe
3+, La
3+Four metal ion species amount of substance sum and Na
2CO
3With the ratio of NaOH amount of substance sum be 0.1: 1, stirring reaction simultaneously, the speed of stirring reaction is 50rpm, keeping the pH value in the reaction process is 8.5;
(3) ageing and oven dry
After step (2) reaction is finished, obtain containing the solution of precipitation, at 15 ℃ of lower ageing 48h, with the solution centrifugal after the ageing, the throw out that separation is obtained is neutral with deionized water rinsing to supernatant liquor repeatedly, and then oven dry obtains product under 70 ℃ of temperature.
(4) use
Taking by weighing the layered di-hydroxyl composite metal oxidate that contains rare earth element joins in the arsenic-containing water solution, the concentration of arsenic is 1mg/L in the arsenic-containing water solution, the concentration that contains the layered di-hydroxyl composite metal oxidate of rare earth element is 0.1g/L, regulate the pH value of gained arsenic-containing water solution after 11.0 take sodium hydroxide solution, place 15 ℃ thermostat container to vibrate 48 hours, oscillation rate is 50rpm, then, measure the concentration of arsenic in the supernatant liquor, according to the concentration difference of arsenic in the water before and after the absorption, determine that sorbent material is to the adsorptive capacity of arsenic element in the water.
Embodiment 4
A kind of preparation method who contains the layered di-hydroxyl composite metal oxidate of rare earth element is characterized in that the method may further comprise the steps:
(1) preparation of solution
With Cu (SO
4)
2, Mg (SO
4)
2, Fe (SO
4)
2And La (NO
3)
3Be dissolved in the deionized water, be mixed with solution 1, Cu in the solution 1
2+Concentration be 100mmolL
-1, Mg
2+Concentration be 20mmolL
-1, Fe
3+Concentration be 30mmolL
-1, La
3+Concentration be 30mmolL
-1Get Na
2CO
3Be dissolved in the deionized water with NaOH, be mixed with solution 2, contain Na in the solution 2
2CO
3Be 800mmolL with the concentration of NaOH
-1
(2) building-up process
Solution 1 and solution 2 are mixed in the deionized water mutually, make Cu
2+, Mg
2+, Fe
3+, La
3+Four metal ion species amount of substance sum and Na
2CO
3With the ratio of NaOH amount of substance sum be 10: 1, stirring reaction simultaneously, the speed of stirring reaction is 1000rpm, keeping the pH value in the reaction process is 13.5;
(3) ageing and oven dry
After step (2) reaction is finished, obtain containing the solution of precipitation, at 90 ℃ of lower ageing 6h, with the solution centrifugal after the ageing, the throw out that separation is obtained is neutral with deionized water rinsing to supernatant liquor repeatedly, and then oven dry obtains product under 250 ℃ of temperature.
(4) use
Taking by weighing the layered di-hydroxyl composite metal oxidate that contains rare earth element joins in the arsenic-containing water solution, the concentration of arsenic is 500mg/L in the arsenic-containing water solution, the concentration that contains the layered di-hydroxyl composite metal oxidate of rare earth element is 0.3g/L, regulate the pH value of gained arsenic-containing water solution after 3 take hydrochloric acid, the thermostat container that places 50 ℃ 2 vibrated 1 hour, oscillation rate is 500rpm, then, measure the concentration of arsenic in the supernatant liquor, according to the concentration difference of arsenic in the water before and after the absorption, determine that sorbent material is to the adsorptive capacity of arsenic element in the water.
Claims (9)
1. a layered di-hydroxyl composite metal oxidate that contains rare earth element is characterized in that, this oxide compound is to contain the simultaneously layered di-hydroxyl composite metal oxidate of cupric, magnesium, three kinds of elements of iron of rare earth element.
2. preparation method who contains the layered di-hydroxyl composite metal oxidate of rare earth element as claimed in claim 1 is characterized in that the method may further comprise the steps:
(1) preparation of solution
The salt of Cu, Mg, Fe and rare earth element is dissolved in the deionized water, is mixed with solution 1, contain Cu in the solution 1
2+, Mg
2+, Fe
3+Be respectively 20mmolL with the concentration of rare earth element
-1～500mmolL
-1Get Na
2CO
3Be dissolved in the deionized water with NaOH, be mixed with solution 2, contain Na in the solution 2
2CO
3Be respectively 400mmolL with the concentration of NaOH
-1～2000mmolL
-1
(2) building-up process
Solution 1 and solution 2 are mixed in the adding deionized water mutually, make Cu
2+, Mg
2+, Fe
3+Four metal ion species amount of substance sum and Na with rare earth element
2CO
3With the ratio of NaOH amount of substance sum be (0.1～10): 1, stirring reaction simultaneously, keeping the pH value in the reaction process is 8.5～13.5;
(3) ageing and oven dry
After step (2) reaction is finished, the solution that obtains, the at a certain temperature ageing regular hour is with the solution centrifugal after the ageing, the throw out that separation is obtained is neutral with deionized water rinsing to supernatant liquor repeatedly, and then oven dry obtains product at a certain temperature.
3. a kind of preparation method who contains the layered di-hydroxyl composite metal oxidate of rare earth element according to claim 2, it is characterized in that, the salt of the described Cu of step (1), Mg, Fe and rare earth element is nitrate, hydrochloride or vitriol, and described rare earth element is La.
4. a kind of preparation method who contains the layered di-hydroxyl composite metal oxidate of rare earth element according to claim 2 is characterized in that, the speed of the described stirring reaction of step (2) is 50～1000rpm.
5. a kind of preparation method who contains the layered di-hydroxyl composite metal oxidate of rare earth element according to claim 2, it is characterized in that, the temperature of the described ageing of step (3) is 15～90 ℃, and the time of ageing is 6h～48h, and bake out temperature is 70 ℃～250 ℃.
6. application that contains the layered di-hydroxyl composite metal oxidate of rare earth element as claimed in claim 1, it is characterized in that, taking by weighing the layered di-hydroxyl composite metal oxidate that contains rare earth element joins in the arsenic-containing water solution, after the pH value with acid or alkaline solution regulator solution, place the thermostat container of the certain temperature certain hour that vibrates, then, measure the concentration of arsenic in the supernatant liquor, according to the concentration difference of arsenic in the water before and after the absorption, determine that sorbent material is to the adsorptive capacity of arsenic element in the water.
7. the application that contains the layered di-hydroxyl composite metal oxidate of rare earth element according to claim 6, it is characterized in that, the concentration range of arsenic is 1～500mg/L in the described arsenic-containing water solution, and the described concentration of layered di-hydroxyl composite metal oxidate in arsenic-containing water solution that contains rare earth element is 0.1-0.3g/L.
8. the application that contains the layered di-hydroxyl composite metal oxidate of rare earth element according to claim 6, it is characterized in that, the alkali of the pH of described regulator solution is sodium hydroxide or ammoniacal liquor, and acid is hydrochloric acid, nitric acid or sulfuric acid, and the pH scope of solution is 3.0～11.0.
9. the application that contains the layered di-hydroxyl composite metal oxidate of rare earth element according to claim 6 is characterized in that, the oscillation rate of described thermostat container is 50～500rpm, and duration of oscillation is 1～48 hour, and the vibration temperature is 15～50 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673111A (en) * | 2017-01-10 | 2017-05-17 | 苏州大学 | Method for treating selenate radical containing waste water |
| CN109289857A (en) * | 2018-09-17 | 2019-02-01 | 同济大学 | Rare earth doped layered composite metal hydroxides and its preparation and application |
| CN109437115A (en) * | 2017-08-30 | 2019-03-08 | 上海沪正实业有限公司 | A kind of inorganic infrared barrier pigment and preparation method thereof |
| CN113663639A (en) * | 2021-08-25 | 2021-11-19 | 四川大学 | Preparation method of lanthanum-doped layered double oxide, product and application thereof |
| CN117323958A (en) * | 2023-12-01 | 2024-01-02 | 水利部牧区水利科学研究所 | Nanometer adsorption material and preparation method and application thereof |
| CN117732420A (en) * | 2023-12-20 | 2024-03-22 | 蔚孚科技(丽水)有限公司 | Flaky porous defluorination adsorbent, and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673111A (en) * | 2017-01-10 | 2017-05-17 | 苏州大学 | Method for treating selenate radical containing waste water |
| CN106673111B (en) * | 2017-01-10 | 2020-09-08 | 苏州大学 | Method for treating wastewater containing selenate |
| CN109437115A (en) * | 2017-08-30 | 2019-03-08 | 上海沪正实业有限公司 | A kind of inorganic infrared barrier pigment and preparation method thereof |
| CN109289857A (en) * | 2018-09-17 | 2019-02-01 | 同济大学 | Rare earth doped layered composite metal hydroxides and its preparation and application |
| CN113663639A (en) * | 2021-08-25 | 2021-11-19 | 四川大学 | Preparation method of lanthanum-doped layered double oxide, product and application thereof |
| CN117323958A (en) * | 2023-12-01 | 2024-01-02 | 水利部牧区水利科学研究所 | Nanometer adsorption material and preparation method and application thereof |
| CN117323958B (en) * | 2023-12-01 | 2024-02-13 | 水利部牧区水利科学研究所 | Nanometer adsorption material and preparation method and application thereof |
| CN117732420A (en) * | 2023-12-20 | 2024-03-22 | 蔚孚科技(丽水)有限公司 | Flaky porous defluorination adsorbent, and preparation method and application thereof |
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Application publication date: 20130213 |