CN112871128A - Anion intercalated double-metal hydroxide adsorbent, and preparation method and application thereof - Google Patents
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention provides an anion intercalated double metal hydroxide adsorbent, a preparation method and application thereof, belonging to the technical field of heavy metal adsorption materials. The preparation method comprises the following steps: carrying out hydrothermal reaction on divalent metal magnesium salt, trivalent metal aluminum salt and urea to obtain a precursor MgAl-CO3-LDH; adding nitric acid and sodium nitrate into the precursor to obtain a sample MgAl-NO3‑LDH；MgAl‑NO3And carrying out hydrothermal reaction on the-LDH and sodium phytate hydrate to obtain the double metal hydroxide MgAl-PA-LDH with anion intercalation. Compared with other chelating agents, the MgAl-PA-LDH prepared by the invention has stronger chelation effect and more adsorption with metal ionsThe locus has excellent treatment effect on the sewage containing cadmium ions. The invention is prepared by an ion exchange method and a hydrothermal reaction, and the obtained product has better stability when being used in acid sewage.
Description
Technical Field
The invention relates to the technical field of heavy metal adsorption materials, in particular to an anion intercalated double metal hydroxide adsorbent, and a preparation method and application thereof.
Background
Cadmium is a heavy metal with high toxicity. In recent years, the demand of industries such as plastics, battery manufacturing, mining, papermaking, electroplating and the like for cadmium raw materials is rapidly increased, and simultaneously, a large amount of industrial wastewater containing cadmium is discharged. The discharged cadmium-containing waste water in large quantity can not only cause harm to the ecological environment, but also can produce enrichment in organisms. Particularly, lower aquatic organisms such as algae have strong cadmium enrichment capacity, and further pose serious threats to human health through food chain accumulation, viscera are damaged in a human body in a chronic poisoning mode, so that the liver and the kidney are damaged, and the serious organisms are further killed (environ, polar, 2018,235, 429-434). Therefore, the method is very important for removing cadmium ions in the sewage.
Common methods for removing cadmium include chemical precipitation, membrane separation, ion exchange, and adsorption. Compared with other methods, the adsorption method has the characteristics of simple operation, low cost, environmental friendliness and the like, and is favored by researchers (chem.Eng.J.2015, 273, 240-246). Conventional adsorbents such as zeolite, activated carbon, etc. have limited their applications due to slow adsorption rate, poor selectivity, etc., so that it has become necessary to develop new adsorbents.
Layered Double Hydroxides (LDHs) are two-dimensional Layered anionic clay type compounds. The LDHs are in a structure of a positively charged hydroxide main body layer and an interlayer anion ordered arrangement. Due to the unique layered structure, the characteristics of the chemical components between layers can be regulated and controlled, and the method is widely applied to sewage treatment. However, the inherent active sites of the LDHs materials have weak specific binding capacity to heavy metal ions, and most of the documents adopt interlayer insertion of ideal anions to perform chelation with the heavy metal ions, so as to achieve the purpose of adsorbing the heavy metals (J.Am.chem.Soc.2016,138, 2858-2866; J.Mater.chem.A, 2014,2, 10280-10289; chem.Eng.J.2017,323, 212-223). The intercalation ionic drugs used in these documents are not only expensive and unstable in chemical properties, but also harsh and complex in conditions during the synthesis process, resulting in increased cost, which is not favorable for application.
The phytic acid is a hexaphosphate substituted cyclic acid, the molecular structure of the phytic acid contains 6 phosphate groups, the surface property of the adsorbent can be modified, and the phytic acid is used as a chelating group on the phytic acid to form a stable chelate with heavy metal ions, so that the heavy metal ions in the solution are removed, and the phytic acid is green, environment-friendly and low in cost. CN 106881067B, "a modified hydrotalcite-like adsorbent and applications thereof", describes the study of adsorption of hydrotalcite intercalated with phytate to lead, but a one-step method is used in the synthesis process, which easily causes the instability of the crystal form size of the synthesized adsorbent, and no report on the adsorption of cadmium ions is found. Therefore, the improvement of the phytic acid intercalated LDHs adsorbent and the research on the removal of cadmium ions in sewage are meaningful.
Disclosure of Invention
The invention aims to: aiming at the problems, the invention provides an anion intercalated double metal hydroxide adsorbent, a preparation method and application thereof, and the invention obtains MgAl-NO with a unique molecular structure by an improved method3LDH, and the phytic acid is intercalated between the double metal hydroxide layers, compared with other chelating agents, the double metal hydroxide double metal chelating agent has stronger chelation effect and more adsorption sites with metal ions, and has very excellent effect on treating the sewage containing cadmium ions.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the anion intercalated double metal hydroxide adsorbent comprises the following steps:
(1) weighing a certain amount of soluble divalent metal magnesium salt and soluble trivalent metal aluminum salt, and dissolving in deionized water to obtain a mixed solution A;
(2) adding urea into the mixed solution A obtained in the step (1), uniformly stirring, transferring into a polytetrafluoroethylene reaction kettle, reacting under a hydrothermal condition, centrifugally separating, washing with deionized water, drying in an oven to obtain a sample which is a precursor MgAl-CO3-LDH；
(3) Weighing the precursor MgAl-CO in the step (2)3dissolving-LDH in decarbonized deionized water, adding nitric acid and sodium nitrate, stirring at room temperature in nitrogen atmosphere, and centrifugally separatingSeparating, washing the solid part with de-carbonated deionized water, putting the washed solid part into an oven for drying to obtain a sample of MgAl-NO3-LDH；
(4) MgAl-NO in the step (3)3Mixing LDH and sodium phytate hydrate, and quickly dissolving in decarbonized deionized water to obtain a mixed solution B;
(5) and (3) transferring the mixed solution B in the step (4) into a polytetrafluoroethylene reaction kettle, reacting under a hydrothermal condition, performing centrifugal separation, washing with de-carbonated deionized water, and drying in an oven to obtain the double metal hydroxide MgAl-PA-LDH with the anion intercalation as a sample.
In the invention, the soluble divalent metal magnesium salt and the soluble trivalent metal aluminum salt in the step (1) are magnesium nitrate and aluminum nitrate respectively, and the molar ratio of the magnesium nitrate to the aluminum nitrate is preferably 1-4: 1.
In the present invention, the molar ratio of the urea in the step (2) to the trivalent metal aluminum salt added in the step (1) is preferably 1:1 to 5.
In the present invention, preferably, the hydrothermal conditions in step (2) are a hydrothermal temperature of 100 to 140 ℃ and a hydrothermal time of 24 to 48 hours.
In the present invention, preferably, MgAl-CO described in the step (3)3The mass-volume ratio of the-LDH to the decarbonized deionized water is 0.1g: 50-100 mL.
In the invention, preferably, the molar concentration of the sodium nitrate added into the decarbonized deionized water in the step (3) is 1-2M, and the molar concentration of the nitric acid added into the decarbonized deionized water is 1-5 mM.
In the present invention, preferably, MgAl-NO in the step (4)3The mass mol ratio of the-LDH to the sodium phytate hydrate is 0.1g: 2.5-7.5 mmol, and MgAl-NO3The mass-volume ratio of the-LDH to the decarbonized deionized water is 0.1g: 24-72 mL.
In the invention, preferably, the hydrothermal condition in the step (5) is that the hydrothermal temperature is 80-120 ℃ and the hydrothermal time is 8-12 hours.
The invention also protects the anion intercalated double metal hydroxide adsorbent prepared by the preparation method.
Researches show that the adsorption capacity of MgAl-PA-LDH prepared by the method to cadmium ions in sewage reaches 92.3mg/g, and the removal rate is about 95%. The method has larger adsorption capacity and higher removal efficiency on metal ion cadmium in the sewage, and can be applied to the field of sewage treatment, so the invention also protects the application of the anion intercalated double metal hydroxide adsorbent prepared by the preparation method in the aspect of being used as a sewage treatment agent.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
(1) the invention uses MgAl-CO3The LDH is precursor and MgAl-NO with unique molecular structure is prepared by ion exchange method and hydrothermal reaction3LDH and MgAl-PA-LDH nano-adsorbent is further synthesized, the obtained crystal grows completely, the grain size is large, compared with other chelating agents, the nano-adsorbent has stronger chelation with metal ions and more adsorption sites, and the nano-adsorbent has excellent effect on treating the sewage containing cadmium ions.
(2) The preparation method of the invention is convenient to operate, the raw materials are cheap and easy to obtain, and the industrial production and popularization and use are easy.
Drawings
FIG. 1 is a powder diffraction (XRD) pattern of MgAl-PA-LDH of example 2 of the present invention.
FIG. 2 is a Scanning Electron Microscope (SEM) image of MgAl-PA-LDH of example 2 of the present invention.
FIG. 3 is a graph showing the adsorption kinetics of MgAl-PA-LDH to cadmium in example 2 of the present invention.
FIG. 4 is [ Mg ] of comparative example 12Al(OH)2](Ph)0.42·4.87H2Adsorption kinetics curve of O to cadmium.
FIG. 5 is the adsorption isotherm of MgAl-PA-LDH of the present invention for cadmium.
FIG. 6 is [ Mg ] of comparative example 12Al(OH)2](Ph)0.42·4.87H2Adsorption isotherm of O on cadmium.
Fig. 7 shows the removal rate of cadmium under acidic conditions for the adsorbents prepared in example and comparative example 1.
Detailed Description
In order that the invention may be more clearly expressed, the invention will now be further described by way of specific examples.
First, preparation example
Example 1
The preparation method of the anion intercalated double metal hydroxide adsorbent comprises the following steps:
(1) weighing 2.5642g of soluble magnesium nitrate as a divalent metal magnesium salt and 1.6224g of soluble aluminum nitrate as a trivalent metal aluminum salt, and dissolving in 50mL of deionized water to obtain a mixed solution A;
(2) adding urea into the mixed solution A in the step (1), wherein the molar ratio of the urea to the trivalent metal aluminum salt added in the step (1) is 1:1, uniformly stirring, transferring into a polytetrafluoroethylene reaction kettle, reacting under the hydrothermal condition that the hydrothermal temperature is 100 ℃ and the hydrothermal time is 48 hours, centrifugally separating, washing with deionized water, drying in an oven to obtain a sample which is a precursor MgAl-CO3-LDH；
(3) Weighing 0.1g of precursor MgAl-CO in the step (2)3dissolving-LDH in 50mL decarbonized deionized water, adding nitric acid and sodium nitrate, enabling the molar concentration of the sodium nitrate added in the decarbonized deionized water to be 1M, enabling the molar concentration of the nitric acid added in the decarbonized deionized water to be 1mM, stirring in a nitrogen atmosphere at room temperature, performing centrifugal separation, washing a solid part with the decarbonized deionized water, putting the solid part into an oven, and drying to obtain a sample of MgAl-NO3-LDH；
(4) Mixing 0.1g of MgAl-NO obtained in the step (3)3Mixing the-LDH and 2.5mmol of sodium phytate hydrate, and quickly dissolving the mixture in 24mL of decarbonized deionized water to obtain a mixed solution B;
(5) and (3) transferring the mixed solution B in the step (4) into a polytetrafluoroethylene reaction kettle, reacting under the hydrothermal condition that the hydrothermal temperature is 80 ℃ and the hydrothermal time is 12 hours, centrifugally separating, washing with de-carbonated deionized water, and drying in an oven to obtain the double metal hydroxide MgAl-PA-LDH with the anion intercalation.
The removal rate of the MgAl-PA-LDH prepared by the embodiment on cadmium ions in sewage is about 94.1%.
Example 2
The preparation method of the anion intercalated double metal hydroxide adsorbent comprises the following steps:
(1) weighing 2.5642g of soluble magnesium nitrate as a divalent metal magnesium salt and 1.8756g of soluble aluminum nitrate as a trivalent metal aluminum salt, and dissolving in 50mL of deionized water to obtain a mixed solution A;
(2) adding urea into the mixed solution A in the step (1), wherein the molar ratio of the urea to the trivalent metal aluminum salt added in the step (1) is 1:3, uniformly stirring, transferring into a polytetrafluoroethylene reaction kettle, reacting under the hydrothermal condition that the hydrothermal temperature is 120 ℃ and the hydrothermal time is 36 hours, centrifugally separating, washing with deionized water, drying in an oven to obtain a sample which is a precursor MgAl-CO3-LDH；
(3) Weighing 0.1g of precursor MgAl-CO in the step (2)3dissolving-LDH in 80mL of decarbonized deionized water, adding nitric acid and sodium nitrate, enabling the molar concentration of the sodium nitrate added in the decarbonized deionized water to be 1.5M, enabling the molar concentration of the nitric acid added in the decarbonized deionized water to be 3mM, stirring in a nitrogen atmosphere at room temperature, performing centrifugal separation, washing a solid part with the decarbonized deionized water, putting the solid part into an oven, and drying to obtain a sample of MgAl-NO3-LDH；
(4) Mixing 0.1g of MgAl-NO obtained in the step (3)3Mixing LDH and 5mmol sodium phytate hydrate, and quickly dissolving in 48mL decarbonized deionized water to obtain a mixed solution B;
(5) and (3) transferring the mixed solution B in the step (4) into a polytetrafluoroethylene reaction kettle, reacting under the hydrothermal condition that the hydrothermal temperature is 100 ℃ and the hydrothermal time is 10 hours, centrifugally separating, washing with de-carbonated deionized water, and drying in an oven to obtain the double metal hydroxide MgAl-PA-LDH with the anion intercalation.
The removal rate of the MgAl-PA-LDH prepared by the embodiment on cadmium ions in sewage is about 95%.
Example 3
The preparation method of the anion intercalated double metal hydroxide adsorbent comprises the following steps:
(1) weighing 2.5642g of soluble magnesium nitrate as a divalent metal magnesium salt and 1.6224g of soluble aluminum nitrate as a trivalent metal aluminum salt, and dissolving in 50mL of deionized water to obtain a mixed solution A;
(2) adding urea into the mixed solution A in the step (1), wherein the molar ratio of the urea to the trivalent metal aluminum salt added in the step (1) is 1:5, uniformly stirring, transferring into a polytetrafluoroethylene reaction kettle, reacting under the hydrothermal condition that the hydrothermal temperature is 140 ℃ and the hydrothermal time is 24 hours, centrifugally separating, washing with deionized water, drying in an oven to obtain a sample which is a precursor MgAl-CO3-LDH；
(3) Weighing 0.1g of precursor MgAl-CO in the step (2)3Dissolving LDH in 100ml decarbonized deionized water, adding nitric acid and sodium nitrate, enabling the molar concentration of the sodium nitrate added in the decarbonized deionized water to be 2M, enabling the molar concentration of the nitric acid added in the decarbonized deionized water to be 5mM, stirring in a nitrogen atmosphere at room temperature, performing centrifugal separation, washing a solid part with the decarbonized deionized water, putting the solid part into an oven, and drying to obtain a sample of MgAl-NO3-LDH；
(4) Mixing 0.1g of MgAl-NO obtained in the step (3)3mixing-LDH and 7.5mmol sodium phytate hydrate, and quickly dissolving in 72mL decarbonized deionized water to obtain a mixed solution B;
(5) and (3) transferring the mixed solution B in the step (4) into a polytetrafluoroethylene reaction kettle, reacting under the hydrothermal condition that the hydrothermal temperature is 120 ℃ and the hydrothermal time is 8 hours, centrifugally separating, washing with de-carbonated deionized water, and drying in an oven to obtain the double metal hydroxide MgAl-PA-LDH with the anion intercalation.
The removal rate of the MgAl-PA-LDH prepared by the embodiment on cadmium ions in sewage is about 94.5%.
Comparative example 1
1. 5.128g of magnesium nitrate and 3.751g of aluminum nitrate were weighed and dissolved in 70mL of boiled deionized water, the pH of the solution was maintained at about 10 with ammonia water, the solution was crystallized at 120 ℃ for 10 hours, washed with water and centrifuged, and dried at 60 ℃ for 24 hours to obtain a sample, [ Mg ]2Al(OH)2](NO3)5·5.6H2O。
2. The obtained Mg2Al-NO3Adding LDH into 100mL hot water solution containing potassium phytate 0.15M, stirring in nitrogen atmosphere at 80 deg.C in thermostatic water bath for 12 hr, and centrifuging to dry to obtain modified hydrotalcite adsorbent with chemical formula of [ Mg2Al(OH)2](Ph)0.42·4.87H2O。
Second, product confirmation
MgAl-CO obtained in examples 1-33-LDH、MgAl-NO3the-LDH and the MgAl-PA-LDH products are respectively subjected to X-ray powder diffraction analysis, and the characterization of X-ray powder diffraction structures of the three materials shows that the MgAl-PA-LDH has obvious characteristic diffraction peaks of LDH, compared with MgAl-CO3LDH and MgAl-NO3LDH, characteristic peak at (003) plane shifted towards low angles, indicating that phytic acid is inserted into the adsorbent, leading to a broadening of the interlamellar spacing of the material. Wherein MgAl-CO is present in example 23-LDH、MgAl-NO3The X-ray powder diffraction patterns of-LDH and MgAl-PA-LDH are shown in FIG. 1.
SEM scanning electron microscope analysis of the adsorbent MgAl-PA-LDH prepared in examples 1-3 shows that the crystal form is complete and hexagonal, the size is large, and the basic microscopic morphology of LDH is maintained. Wherein, the SEM picture of the MgAl-PA-LDH prepared in example 2 is shown in figure 2.
Third, testing the adsorption performance
1. 10Mg of the adsorbents prepared in example 2 and comparative example 1 were weighed, added to 30mL of a solution containing cadmium ions at a concentration of 10ppm, shaken at a constant temperature of 25 ℃, sampled at different times within 0 to 24 hours, and the obtained sample was subjected to ICP-MS to determine the concentration of cadmium ions, and the adsorption kinetics curve of MgAl-PA-LDH of example 2 is shown in FIG. 3, and [ Mg-PA-LDH of comparative example 1 is shown in FIG. 32Al(OH)2](Ph)0.42·4.87H2The adsorption kinetics curve of O is shown in FIG. 4, and can be obtained from FIG. 3, when the adsorption equilibrium is reached, the removal rate of cadmium ions by the adsorbent prepared in example 2 is 95.2%. As can be seen from FIG. 4, when the adsorption equilibrium is reached, the adsorption prepared in comparative example 1The removal rate of the cadmium ions by the adhesive is 79.1 percent.
2. 20Mg of the MgAl-PA-LDH adsorbent prepared in the above example 2 and the comparative example 1 are respectively weighed and placed in 30mL of cadmium ion-containing solution with the concentration of 5-800 ppm, the solution is shaken at a constant temperature of 25 ℃ for 24h, the concentration of cadmium ions in the solution after reaction equilibrium is measured by ICP-MS, the adsorption isotherm of the MgAl-PA-LDH of the example 2 is drawn as shown in FIG. 5, and the [ Mg-PA-LDH of the comparative example 1 is drawn as shown in FIG. 12Al(OH)2](Ph)0.42·4.87H2As shown in FIG. 6, the maximum adsorption capacity of the adsorbent of example 2 reached 92.3mg/g and the maximum adsorption capacity of the adsorbent of comparative example 1 reached 80.6mg/g after the equilibrium reaction. MgAl-CO higher than that reported in literature3Maximum adsorption capacity of LDH for cadmium ions (45.6mg/g) (j.hazard. mater. 2015,299, 42-49). The MgAl-PA-LDH has better adsorption effect on cadmium ions.
Fourth, stability test
To examine the stability of MgAl-PA-LDH of the present invention in acidic wastewater, MgAl-PA-LDH prepared in example 2 of the present invention and [ Mg ] prepared in comparative example 1 were used2Al(OH)2](Ph)0.42·4.87H2The adsorption performance of O in cadmium-containing acidic sewage is tested, and the specific experimental method is as follows:
20mg of the adsorbents prepared in example 2 and comparative example 1 were weighed, respectively, and added to 20mL of a cadmium ion-containing solution having a pH of 10ppm, and the mixture was shaken at a constant temperature of 25 ℃ for 24 hours, and the concentration of cadmium ions in the solution after the reaction equilibrium was measured by ICP-MS. As shown in fig. 7, the removal rate of example 2 was 95.38%, and the performance of adsorbing cadmium was not affected. The removal rate of cadmium by the adsorbent of the comparative example 1 is obviously reduced, and it can be seen that the MgAl-PA-LDH prepared in the embodiment 2 of the invention is compared with the [ Mg ] prepared in the comparative example 12Al(OH)2](Ph)0.42·4.87H2The adsorption performance of O under acidic condition is more stable, and the O-containing composite material has better practical value.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.
Claims (10)
1. The preparation method of the anion intercalated double metal hydroxide adsorbent is characterized by comprising the following steps:
(1) weighing a certain amount of soluble divalent metal magnesium salt and soluble trivalent metal aluminum salt, and dissolving in deionized water to obtain a mixed solution A;
(2) adding urea into the mixed solution A obtained in the step (1), uniformly stirring, transferring into a polytetrafluoroethylene reaction kettle, reacting under a hydrothermal condition, centrifugally separating, washing with deionized water, drying in an oven to obtain a sample which is a precursor MgAl-CO3-LDH；
(3) Weighing the precursor MgAl-CO in the step (2)3dissolving-LDH in decarbonized deionized water, adding nitric acid and sodium nitrate, stirring at room temperature in a nitrogen atmosphere, performing centrifugal separation, washing a solid part with decarbonized deionized water, and drying in an oven to obtain a sample MgAl-NO3-LDH；
(4) MgAl-NO in the step (3)3Mixing LDH and sodium phytate hydrate, and quickly dissolving in decarbonized deionized water to obtain a mixed solution B;
(5) and (3) transferring the mixed solution B in the step (4) into a polytetrafluoroethylene reaction kettle, reacting under a hydrothermal condition, performing centrifugal separation, washing with de-carbonated deionized water, and drying in an oven to obtain the double metal hydroxide MgAl-PA-LDH with the anion intercalation as a sample.
2. The method of preparing an anion intercalated double metal hydroxide adsorbent according to claim 1, characterized in that: the soluble divalent metal magnesium salt and the soluble trivalent metal aluminum salt in the step (1) are respectively magnesium nitrate and aluminum nitrate, and the molar ratio of the magnesium nitrate to the aluminum nitrate is 1-4: 1.
3. The method of preparing an anion intercalated double metal hydroxide adsorbent according to claim 1, characterized in that: the molar ratio of the urea in the step (2) to the trivalent metal aluminum salt added in the step (1) is 1: 1-5.
4. The method of preparing an anion intercalated double metal hydroxide adsorbent according to claim 1, characterized in that: the hydrothermal condition in the step (2) is that the hydrothermal temperature is 100-140 ℃ and the hydrothermal time is 24-48 hours.
5. The method of preparing an anion intercalated double metal hydroxide adsorbent according to claim 1, characterized in that: MgAl-CO described in step (3)3The mass-volume ratio of the-LDH to the decarbonized deionized water is 0.1g: 50-100 mL.
6. The method of preparing an anion intercalated double metal hydroxide adsorbent according to claim 1, characterized in that: and (4) adding sodium nitrate into de-carbonated deionized water to obtain a molar concentration of 1-2M, and adding nitric acid into the de-carbonated deionized water to obtain a molar concentration of 1-5 mM.
7. The method of preparing an anion intercalated double metal hydroxide adsorbent according to claim 1, characterized in that: MgAl-NO described in step (4)3The mass mol ratio of the-LDH to the sodium phytate hydrate is 0.1g: 2.5-7.5 mmol, and MgAl-NO3The mass-volume ratio of the-LDH to the decarbonized deionized water is 0.1g: 24-72 mL.
8. The method of preparing an anion intercalated double metal hydroxide adsorbent according to claim 1, characterized in that: the hydrothermal condition in the step (5) is that the hydrothermal temperature is 80-120 ℃ and the hydrothermal time is 8-12 hours.
9. The anion-intercalated double metal hydroxide adsorbent prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the anion-intercalated double metal hydroxide adsorbent prepared by the preparation method according to any one of claims 1 to 8 as a sewage treatment agent.
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| CN113413864A (en) * | 2021-07-30 | 2021-09-21 | 宁夏医科大学 | Layered double-metal hydroxide complex for adsorbing heavy metal ions and preparation method and application thereof |
| CN113666427A (en) * | 2021-09-01 | 2021-11-19 | 中国地质大学（武汉） | Transition metal layered double hydroxide modified by phytic acid and preparation method and application thereof |
| CN113929492A (en) * | 2021-10-15 | 2022-01-14 | 成都工业学院 | Preparation method of hydrotalcite-like composite material for phosphorus recovery, and product and application thereof |
| CN114558552A (en) * | 2022-04-06 | 2022-05-31 | 北京师范大学 | LDH composite material and preparation method and application thereof |
| CN115845792A (en) * | 2022-10-21 | 2023-03-28 | 黑龙江省科学院高技术研究院 | Preparation method and application of transition metal doped magnesium-aluminum layered double hydroxide material |
| CN116081671A (en) * | 2023-01-17 | 2023-05-09 | 广东华特气体股份有限公司 | Porous double-metal hydroxide and preparation method and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012081A (en) * | 2007-01-30 | 2007-08-08 | 浙江工商大学 | Method of reducing heavy metal in mussel boiling liquid by phytic acid |
| CN101649198A (en) * | 2009-09-17 | 2010-02-17 | 北京化工大学 | Lucigen cation and brucite composite luminescence film and preparation method thereof |
| CN101972631A (en) * | 2010-09-17 | 2011-02-16 | 北京化工大学 | Multilevel-structure hydrotalcite adsorbent and preparation method thereof |
| CN102502519A (en) * | 2011-11-03 | 2012-06-20 | 浙江大学 | Method for preparing peeled layered material/ carbon nano tube complex in aqueous solution |
| CN104307492A (en) * | 2014-10-28 | 2015-01-28 | 郑州轻工业学院 | Mg2Al-LS-LDH composite material as well as preparation method and application of composite material |
| CN104923154A (en) * | 2015-05-07 | 2015-09-23 | 北京化工大学 | Hexagonal sheet magnetic metal/metal oxide/carbon nanocomposite adsorbing material and preparation method therefor |
| CN105924468A (en) * | 2016-05-03 | 2016-09-07 | 首都师范大学 | Novel hydrogel prepared from phytic acid and soluble metal salt and preparing method thereof |
| CN106881067A (en) * | 2017-04-24 | 2017-06-23 | 北京化工大学 | A kind of modified houghite adsorbent and its application |
-
2021
- 2021-01-19 CN CN202110071285.8A patent/CN112871128A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012081A (en) * | 2007-01-30 | 2007-08-08 | 浙江工商大学 | Method of reducing heavy metal in mussel boiling liquid by phytic acid |
| CN101649198A (en) * | 2009-09-17 | 2010-02-17 | 北京化工大学 | Lucigen cation and brucite composite luminescence film and preparation method thereof |
| CN101972631A (en) * | 2010-09-17 | 2011-02-16 | 北京化工大学 | Multilevel-structure hydrotalcite adsorbent and preparation method thereof |
| CN102502519A (en) * | 2011-11-03 | 2012-06-20 | 浙江大学 | Method for preparing peeled layered material/ carbon nano tube complex in aqueous solution |
| CN104307492A (en) * | 2014-10-28 | 2015-01-28 | 郑州轻工业学院 | Mg2Al-LS-LDH composite material as well as preparation method and application of composite material |
| CN104923154A (en) * | 2015-05-07 | 2015-09-23 | 北京化工大学 | Hexagonal sheet magnetic metal/metal oxide/carbon nanocomposite adsorbing material and preparation method therefor |
| CN105924468A (en) * | 2016-05-03 | 2016-09-07 | 首都师范大学 | Novel hydrogel prepared from phytic acid and soluble metal salt and preparing method thereof |
| CN106881067A (en) * | 2017-04-24 | 2017-06-23 | 北京化工大学 | A kind of modified houghite adsorbent and its application |
Non-Patent Citations (1)
| Title |
|---|
| 庄海燕等: "植酸对镉污染土壤中镉解吸的影响", 《四川环境》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113413864A (en) * | 2021-07-30 | 2021-09-21 | 宁夏医科大学 | Layered double-metal hydroxide complex for adsorbing heavy metal ions and preparation method and application thereof |
| CN113666427A (en) * | 2021-09-01 | 2021-11-19 | 中国地质大学（武汉） | Transition metal layered double hydroxide modified by phytic acid and preparation method and application thereof |
| CN113666427B (en) * | 2021-09-01 | 2022-05-24 | 中国地质大学（武汉） | Transition metal layered double hydroxide modified by phytic acid and preparation method and application thereof |
| CN113929492A (en) * | 2021-10-15 | 2022-01-14 | 成都工业学院 | Preparation method of hydrotalcite-like composite material for phosphorus recovery, and product and application thereof |
| CN114558552A (en) * | 2022-04-06 | 2022-05-31 | 北京师范大学 | LDH composite material and preparation method and application thereof |
| CN115845792A (en) * | 2022-10-21 | 2023-03-28 | 黑龙江省科学院高技术研究院 | Preparation method and application of transition metal doped magnesium-aluminum layered double hydroxide material |
| CN115845792B (en) * | 2022-10-21 | 2024-02-23 | 黑龙江省科学院高技术研究院 | Preparation method and application of transition metal doped magnesium-aluminum layered double hydroxide material |
| CN116081671A (en) * | 2023-01-17 | 2023-05-09 | 广东华特气体股份有限公司 | Porous double-metal hydroxide and preparation method and application thereof |
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