CN114162945A - Meta-aluminate intercalated magnesium-iron type hydrotalcite and preparation method thereof - Google Patents
Meta-aluminate intercalated magnesium-iron type hydrotalcite and preparation method thereof Download PDFInfo
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- CN114162945A CN114162945A CN202111348799.XA CN202111348799A CN114162945A CN 114162945 A CN114162945 A CN 114162945A CN 202111348799 A CN202111348799 A CN 202111348799A CN 114162945 A CN114162945 A CN 114162945A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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Abstract
The invention relates to a meta-aluminate intercalated magnesium-iron type hydrotalcite and a preparation method thereof, wherein the method comprises the following steps: (1) preparing a magnesium-iron mixed salt solution: adding magnesium salt and ferric salt into deionized water, and stirring to obtain a magnesium-iron mixed salt solution; (2) preparing an aluminum-sodium mixed alkali solution: adding metaaluminate and alkali into deionized water, and stirring to obtain an aluminum-sodium mixed alkali solution; (3) preparing a suspension: dripping a magnesium-iron mixed salt solution and an aluminum-sodium mixed alkali solution into deionized water at the same time, stirring, controlling the pH value of the solution to be 8-13, and continuously heating and stirring after dripping is finished to obtain a suspension; (4) aging and crystallizing: standing the suspension, and then heating, aging and crystallizing to obtain a crystal precipitate; (5) and filtering, washing and drying the crystallized precipitate to obtain the meta-aluminate intercalated magnesium-iron hydrotalcite. Compared with the prior art, the invention has the advantages of wide material source, simplicity, reliability, no pollution, low preparation cost and the like.
Description
Technical Field
The invention relates to the field of chemical material preparation, and particularly relates to a meta-aluminate intercalated magnesium-iron hydrotalcite and a preparation method thereof.
Background
Hydrotalcite is a layered double hydroxide having a layered structure and interlayer ions, and has applications in various fields such as medicine, ion exchange, adsorption, and the like due to the properties of interlayer anion exchangeability, thermal stability, memory effect, flame retardancy, catalytic performance, and infrared absorption performance.
The hydrotalcite may be synthesized by a variety of methods, including hydrothermal synthesis, low saturation coprecipitation, high saturation coprecipitation, ion synthesis, and calcination recovery. Among them, the low-maintenance and precipitation method is generally used because of its simple operation and low risk.
The hydrotalcite has the characteristics of no toxicity, low preparation cost, no harm to the environment, better anion removal performance and the like. However, in the adsorption aspect, compared with materials such as activated carbon, hydrotalcite has weaker adsorption capacity and poorer regenerability, and the types of pollutants capable of being adsorbed are limited to anionic pollutants, so that the application of hydrotalcite in the adsorption aspect is greatly limited.
The method for enhancing the adsorption performance of hydrotalcite by inserting other anions into the interlayer structure of the hydrotalcite material is a popular modification method, but because the intercalated anions have various types and are easy to cause secondary pollution after entering a water body through ion exchange, the selection of the intercalated anions is greatly limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the meta-aluminate intercalated magnesium-iron hydrotalcite with wide material source, simplicity, reliability, no pollution and low preparation cost and the preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a method for preparing a meta-aluminate intercalated magnesium-iron hydrotalcite, which takes meta-aluminate as an intercalation material, the prepared hydrotalcite has good adsorption performance, and the meta-aluminate can continue flocculating pollutants in water after entering the water body after ion exchange, and the specific scheme is as follows:
a method for preparing meta-aluminate intercalated magnesium-iron type hydrotalcite comprises the following steps:
(1) preparing a magnesium-iron mixed salt solution: adding magnesium salt and ferric salt into deionized water, and stirring to obtain a magnesium-iron mixed salt solution;
(2) preparing an aluminum-sodium mixed alkali solution: adding metaaluminate and alkali into deionized water, and stirring to obtain an aluminum-sodium mixed alkali solution;
(3) preparing a suspension: dripping a magnesium-iron mixed salt solution and an aluminum-sodium mixed alkali solution into deionized water at the same time, stirring, controlling the pH value of the solution to be 8-13, and continuously heating and stirring after dripping is finished to obtain a suspension;
(4) aging and crystallizing: standing the suspension, and then heating, aging and crystallizing to obtain a crystal precipitate;
(5) and filtering, washing and drying the crystallized precipitate to obtain the meta-aluminate intercalated magnesium-iron hydrotalcite.
Furthermore, in the magnesium salt and the iron salt, the molar ratio of magnesium to iron is (2-4): 1.
Furthermore, in the magnesium salt and the iron salt, the molar ratio of magnesium to iron is 3: 1.
Furthermore, in the meta-aluminate and the alkali, the molar ratio of aluminum to hydroxide radical is (0.5-2): 1.
Further, in the meta-aluminate and the alkali, the molar ratio of aluminum to hydroxide radical is 1: 1.
Furthermore, in the suspension, the volume ratio of the magnesium-iron mixed salt solution to the aluminum-sodium mixed alkali solution is (0.4-0.6): 1.
Further, the heating and stirring temperature is 80-90 ℃, and the time is 1.5-2.5 h; the stirring speed is 800-1200 r/min.
Further, the temperature of the heating, aging and crystallization is 60-70 ℃, and the time is 20-24 h.
Further, the drying temperature is 110-.
The meta-aluminate intercalated magnesium-iron hydrotalcite prepared by the method.
Compared with the prior art, the meta-aluminate intercalated magnesium-iron hydrotalcite prepared by the invention has larger specific surface area and pore volume and smaller pore diameter, which indicates that the meta-aluminate intercalated magnesium-iron hydrotalcite prepared by the invention contains more pore structures and can provide more active sites for adsorption. The intercalated meta-aluminate enters a water body after ion exchange with anion pollutants in the water, and can generate aluminum hydroxide precipitate under the acidic or neutral condition and flocculate the pollutants, so that the meta-aluminate intercalated magnesium-iron hydrotalcite has the characteristics of no toxicity, no harm, no halogen and environmental protection.
Drawings
FIG. 1 is a scanning perspective view of an SEM of example 3;
FIG. 2 is a scanning overview of BET of example 3;
FIG. 3 is a scanning observation of XRD of example 3;
FIG. 4 is a scan perspective of XPS of example 3;
FIG. 5 is a graph of a kinetic model of the adsorbed bromate of example 3 and comparative example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.
A method for preparing meta-aluminate intercalated magnesium-iron type hydrotalcite comprises the following steps:
(1) preparing a magnesium-iron mixed salt solution: adding magnesium salt and ferric salt into deionized water, and stirring to obtain a magnesium-iron mixed salt solution; in the magnesium salt and the iron salt, the molar ratio of magnesium to iron is (2-4) to 1; magnesium salts include magnesium chloride hexahydrate, iron salts include ferric nitrate nonahydrate;
(2) preparing an aluminum-sodium mixed alkali solution: adding metaaluminate and alkali into deionized water, and stirring to obtain an aluminum-sodium mixed alkali solution; in the meta-aluminate and the alkali, the molar ratio of aluminum to hydroxide radical is (0.5-2) to 1; the meta-aluminate comprises sodium meta-aluminate, and the alkali comprises sodium hydroxide;
(3) preparing a suspension: dripping a magnesium-iron mixed salt solution and an aluminum-sodium mixed alkali solution into deionized water at the same time, stirring, controlling the pH value of the solution to be 8-13, and continuously heating and stirring after dripping is finished to obtain a suspension; in the suspension, the volume ratio of the magnesium-iron mixed salt solution to the aluminum-sodium mixed alkali solution is (0.4-0.6) to 1, wherein the heating and stirring temperature is 80-90 ℃, and the time is 1.5-2.5 h; the stirring speed is 800-1200 r/min;
(4) aging and crystallizing: standing the suspension, and then heating, aging and crystallizing to obtain a crystal precipitate; wherein the temperature for heating, aging and crystallizing is 60-70 ℃, and the time is 20-24 h;
(5) and filtering, washing and drying the crystallized precipitate to obtain the meta-aluminate intercalated magnesium-iron hydrotalcite. Wherein the drying temperature is 110-.
Example 1
A method for preparing meta-aluminate intercalated magnesium-iron type hydrotalcite comprises the following steps:
(1) preparing a mixed acid solution and a mixed alkali solution: 12.857g of magnesium chloride hexahydrate and 10g of ferric nitrate nonahydrate are weighed, 100ml of deionized water is added, stirred and dissolved completely, and then the mixture is kept stand for 10 min; weighing 2g of sodium metaaluminate and 4g of sodium hydroxide, adding 200ml of deionized water, stirring for dissolving, and standing for 10 min.
(2) Preparing a suspension of the mixed acid solution and the mixed alkali solution: adding 100ml of deionized water into a beaker, stirring, keeping the temperature at room temperature, dropwise adding the prepared mixed acid solution and mixed alkali solution into the beaker at a constant speed, and keeping the pH of the solution at about 8. The volume ratio of the magnesium-iron mixed salt solution to the aluminum-sodium mixed alkali solution is about 0.5: 1.
(3) Aging and crystallizing: after the end of the dropwise addition, the temperature was heated to 85 ℃ and stirring was continued for 2 h. After 2h, stopping stirring, controlling the temperature at 60 ℃, standing, and aging and crystallizing for 20 h.
(4) Filtering, washing and drying: and after aging and crystallization, filtering and precipitating by using a vacuum pump, washing the precipitate by using deionized water until the precipitate is neutral, and then baking and precipitating for 2 hours by using an oven at the temperature of 120 ℃ to obtain the meta-aluminate intercalated magnesium-iron type hydrotalcite.
Example 2
A method for preparing meta-aluminate intercalated magnesium-iron type hydrotalcite comprises the following steps:
(1) preparing a mixed acid solution and a mixed alkali solution: 12.857g of magnesium chloride hexahydrate and 10g of ferric nitrate nonahydrate are weighed, 100ml of deionized water is added, stirred and dissolved completely, and then the mixture is kept stand for 10 min; weighing 4.1g of sodium metaaluminate and 5g of sodium hydroxide, adding 200ml of deionized water, stirring for dissolving, and standing for 10 min.
(2) Preparing a suspension of the mixed acid solution and the mixed alkali solution: adding 100ml of deionized water into a beaker, stirring, keeping the temperature at room temperature, dropwise adding the prepared mixed acid solution and mixed alkali solution into the beaker at a constant speed, and keeping the pH of the solution at about 8.5. The volume ratio of the magnesium-iron mixed salt solution to the aluminum-sodium mixed alkali solution is about 0.5: 1.
(3) Aging and crystallizing: after the end of the dropwise addition, the temperature was heated to 85 ℃ and stirring was continued for 2 h. After 2h, stopping stirring, controlling the temperature at 60 ℃, standing, and aging and crystallizing for 21 h.
(4) Filtering, washing and drying: and after aging and crystallization, filtering and precipitating by using a vacuum pump, washing the precipitate by using deionized water until the precipitate is neutral, and then baking and precipitating for 2 hours by using an oven at the temperature of 120 ℃ to obtain the meta-aluminate intercalated magnesium-iron type hydrotalcite.
Example 3
A method for preparing meta-aluminate intercalated magnesium-iron type hydrotalcite comprises the following steps:
(1) preparing a mixed acid solution and a mixed alkali solution: 12.857g of magnesium chloride hexahydrate and 10g of ferric nitrate nonahydrate are weighed, 100ml of deionized water is added, stirred and dissolved completely, and then the mixture is kept stand for 10 min; weighing 6.1g of sodium metaaluminate and 8g of sodium hydroxide, adding 200ml of deionized water, stirring for dissolving, and standing for 10 min.
(2) Preparing a suspension of the mixed acid solution and the mixed alkali solution: adding 100ml of deionized water into a beaker, stirring, keeping the temperature at room temperature, dropwise adding the prepared mixed acid solution and mixed alkali solution into the beaker at a constant speed, and keeping the pH of the solution at about 10. The volume ratio of the magnesium-iron mixed salt solution to the aluminum-sodium mixed alkali solution is about 0.5: 1.
(3) Aging and crystallizing: after the end of the dropwise addition, the temperature was heated to 85 ℃ and stirring was continued for 2 h. After 2h, stopping stirring, controlling the temperature at 60 ℃, standing, and aging and crystallizing for 22 h.
(4) Filtering, washing and drying: and after aging and crystallization, filtering and precipitating by using a vacuum pump, washing the precipitate by using deionized water until the precipitate is neutral, and then baking and precipitating for 2 hours by using an oven at the temperature of 120 ℃ to obtain the meta-aluminate intercalated magnesium-iron type hydrotalcite.
Through electron microscope (SEM) scanning and pore size scanning (BET) observation, the mean pore size of the meta-aluminate intercalated ferrimagnesium hydrotalcite material prepared by the invention is 8.0023 nanometers, the pore volume is 0.2824 cubic centimeters per gram, and the specific surface area is 136.9655 square meters per gram, which is shown in figure 1-2; according to XRD scanning observation, the hydrotalcite material with the meta-aluminate intercalated magnesium iron type has characteristic peaks of (003), (006) and (009), and conforms to a hydrotalcite structure, and the meta-aluminate intercalated is successful, as shown in figure 3; XPS scanning observation shows that the meta-aluminate intercalated ferrimagnesium hydrotalcite material prepared by the invention contains aluminum element, which shows that the meta-aluminate is successfully intercalated in the hydrotalcite material, and figure 4 shows.
The prepared meta-aluminate intercalated magnesium-iron type hydrotalcite adopts meta-aluminate intercalation, the meta-aluminate can generate aluminum hydroxide in water after entering the water due to ion exchange, the aluminum hydroxide is a flocculating agent, has the effect of continuous water purification, is harmless to human bodies, and cannot cause secondary pollution to the water.
Comparative example 1
A preparation method of non-intercalated magnesium-iron type hydrotalcite comprises the following steps:
(1) preparing a mixed acid solution and a mixed alkali solution: 12.857g of magnesium chloride hexahydrate and 10g of ferric nitrate nonahydrate are weighed, 100ml of deionized water is added, stirred and dissolved completely, and then the mixture is kept stand for 10 min; 12.72g of sodium bicarbonate and 4.8g of sodium hydroxide are weighed, added with 500ml of deionized water, stirred and dissolved, and kept stand for 10 min.
(2) Preparing a suspension of the mixed acid solution and the mixed alkali solution: adding 100ml of deionized water into a beaker, stirring, keeping the temperature at room temperature, dropwise adding the prepared mixed acid solution and mixed alkali solution into the beaker at a constant speed, and keeping the pH of the solution at about 8.5. The volume ratio of the mixed salt solution to the mixed alkali solution is about 0.5: 1.
(3) Aging and crystallizing: after the end of the dropwise addition, the temperature was heated to 85 ℃ and stirring was continued for 2 h. After 2h, stopping stirring, controlling the temperature at 60 ℃, standing, and aging and crystallizing for 23 h.
(4) Filtering, washing and drying: and after aging and crystallization, filtering and precipitating by using a vacuum pump, washing and precipitating to be neutral by using deionized water, then baking and precipitating for 2 hours by using an oven at 120 ℃, and finally roasting for 5 hours by using a muffle furnace at 500 ℃ to obtain the non-intercalated magnesium-iron type hydrotalcite.
As a result of adsorption to bromate, the equilibrium adsorption capacity of the meta-aluminate intercalated ferrimagnesium hydrotalcite prepared in example 3 was 97.7 mg/g, and the equilibrium adsorption capacity of the non-intercalated ferrimagnesium hydrotalcite in comparative example 1 was 78.03 mg/g, as shown in fig. 5. The result shows that the meta-aluminate intercalated magnesium-iron hydrotalcite prepared by the invention has more active sites for adsorption, and the adsorption effect on bromate is higher than that of non-intercalated magnesium-iron hydrotalcite.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A method for preparing an aluminate intercalated magnesium iron type hydrotalcite is characterized by comprising the following steps:
(1) preparing a magnesium-iron mixed salt solution: adding magnesium salt and ferric salt into deionized water, and stirring to obtain a magnesium-iron mixed salt solution;
(2) preparing an aluminum-sodium mixed alkali solution: adding metaaluminate and alkali into deionized water, and stirring to obtain an aluminum-sodium mixed alkali solution;
(3) preparing a suspension: dripping a magnesium-iron mixed salt solution and an aluminum-sodium mixed alkali solution into deionized water at the same time, stirring, controlling the pH value of the solution to be 8-13, and continuously heating and stirring after dripping is finished to obtain a suspension;
(4) aging and crystallizing: standing the suspension, and then heating, aging and crystallizing to obtain a crystal precipitate;
(5) and filtering, washing and drying the crystallized precipitate to obtain the meta-aluminate intercalated magnesium-iron hydrotalcite.
2. The method for preparing the magnesium iron type hydrotalcite with the intercalation of meta-aluminate radicals according to claim 1, wherein the molar ratio of magnesium to iron in the magnesium salts and the iron salts is (2-4): 1.
3. The method for preparing the magnesium iron type hydrotalcite with the intercalation of meta-aluminate radicals according to claim 2, wherein the molar ratio of magnesium to iron in the magnesium salts and the iron salts is 3: 1.
4. The method for preparing the meta-aluminate intercalated magnesium iron hydrotalcite as claimed in claim 1, wherein the molar ratio of aluminum to hydroxyl in the meta-aluminate to the alkali is (0.5-2) to 1.
5. The method for preparing the meta-aluminate intercalated magnesium iron hydrotalcite as claimed in claim 1, wherein the molar ratio of aluminum to hydroxyl in the meta-aluminate to the alkali is 1: 1.
6. The method for preparing the magnesium iron type hydrotalcite with intercalated metaaluminate radical according to claim 1, wherein the volume ratio of the magnesium-iron mixed salt solution to the aluminum-sodium mixed alkali solution in the suspension is (0.4-0.6): 1.
7. The method for preparing the magnesium iron type hydrotalcite with the intercalation of meta-aluminate radical as claimed in claim 1, wherein the temperature for heating and stirring is 80-90 ℃ and the time is 1.5-2.5 h; the stirring speed is 800-1200 r/min.
8. The method for preparing the magnesium iron type hydrotalcite with the intercalation of meta-aluminate radical as claimed in claim 1, wherein the temperature for heating, aging and crystallization is 60-70 ℃ and the time is 20-24 h.
9. The method for preparing the magnesium iron type hydrotalcite with the intercalation of meta-aluminate according to claim 1, wherein the drying temperature is 110-130 ℃ and the drying time is 1.5-2.5 h.
10. A meta-aluminate intercalated magnesium iron hydrotalcite prepared according to the process of any one of claims 1 to 9.
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| CN115716658A (en) * | 2022-08-23 | 2023-02-28 | 中冶赛迪工程技术股份有限公司 | Method for preparing magnesium-iron hydrotalcite by using metal ions in industrial wastewater |
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