CN114162945B - Metalic aluminate intercalation magnesium-iron hydrotalcite and preparation method thereof - Google Patents
Metalic aluminate intercalation magnesium-iron hydrotalcite and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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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- 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
- C02F1/28—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
- 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
- C02F1/28—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 an meta-aluminate intercalation magnesium-iron 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 magnesium-iron mixed salt solution; (2) preparing an aluminum-sodium mixed alkali solution: adding meta-aluminate and alkali into deionized water, and stirring to obtain aluminum-sodium mixed alkali solution; (3) preparing a suspension: simultaneously dropwise adding a magnesium-iron mixed salt solution and an aluminum-sodium mixed alkali solution into deionized water, stirring, controlling the pH value of the solution to be 8-13, and continuing heating and stirring after the dropwise adding 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) Filtering, washing and drying the crystal precipitate to obtain the metaaluminate intercalation 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, in particular to metaaluminate intercalation magnesium-iron hydrotalcite and a preparation method thereof.
Background
Hydrotalcite is a layered double hydroxide, has 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 exchange, thermal stability, memory effect, flame retardance, catalytic performance and infrared absorption.
The hydrotalcite can be synthesized by various methods, including hydrothermal synthesis, low-saturation coprecipitation, high-saturation coprecipitation, ion synthesis, and calcination recovery. Among them, the low-protection and precipitation method is widely used because of simple operation and low risk.
Hydrotalcite has the characteristics of no toxicity, low preparation cost, no harm to the environment, good anion removal performance and the like. However, in the adsorption aspect, compared with the materials such as activated carbon, hydrotalcite has weak adsorption capacity and poor regenerability, and the types of adsorbable pollutants are limited to anionic pollutants, so that the application of hydrotalcite in the adsorption aspect is greatly limited.
The intercalation of other anions in the interlayer structure of hydrotalcite material enhances the adsorption performance of hydrotalcite, but the intercalation anions are very limited because of various types of anions and easy secondary pollution after entering water body and ion exchange.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the metaaluminate intercalation magnesium-iron hydrotalcite and the preparation method thereof, wherein the metaaluminate intercalation magnesium-iron hydrotalcite has wide material source, simplicity, reliability and no pollution and low preparation cost.
The aim of the invention can be achieved by the following technical scheme:
the invention provides a method for preparing metaaluminate intercalation magnesium-iron hydrotalcite by taking metaaluminate as intercalation material, wherein the prepared hydrotalcite has good adsorption performance, and the metaaluminate can continuously flocculate pollutants in water after entering water after ion exchange, and the specific scheme is as follows:
the preparation process of intercalated magnesium-iron hydrotalcite with metaaluminate includes the following steps:
(1) Preparing a magnesium-iron mixed salt solution: adding magnesium salt and ferric salt into deionized water, and stirring to obtain magnesium-iron mixed salt solution;
(2) Preparing an aluminum-sodium mixed alkali solution: adding meta-aluminate and alkali into deionized water, and stirring to obtain aluminum-sodium mixed alkali solution;
(3) Preparing a suspension: simultaneously dropwise adding a magnesium-iron mixed salt solution and an aluminum-sodium mixed alkali solution into deionized water, stirring, controlling the pH value of the solution to be 8-13, and continuing heating and stirring after the dropwise adding is finished to obtain a suspension;
(4) And (5) aging and crystallizing: standing the suspension, and then heating, aging and crystallizing to obtain a crystal precipitate;
(5) Filtering, washing and drying the crystal precipitate to obtain the metaaluminate intercalation magnesium-iron hydrotalcite.
Further, in the magnesium salt and the ferric salt, the molar ratio of magnesium to iron is (2-4): 1.
Further, in the magnesium salt and the ferric salt, the molar ratio of magnesium to iron is 3:1.
Further, in the meta-aluminate and the alkali, the molar ratio of aluminum to hydroxide is (0.5-2): 1.
Further, in the meta-aluminate and the alkali, the molar ratio of aluminum to hydroxide is 1:1.
Further, 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 temperature of heating and stirring is 80-90 ℃ and the time is 1.5-2.5h; the stirring speed is 800-1200r/min.
Further, the temperature of the heating aging crystallization is 60-70 ℃ and the time is 20-24 hours.
Further, the temperature of the drying is 110-130 ℃ and the time is 1.5-2.5h.
The metaaluminate intercalation 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 metaaluminate enters the water body after ion exchange with anionic pollutants in the water, and can generate aluminum hydroxide sediment under the acidic or neutral condition and flocculate pollutants, so that the metaaluminate intercalated magnesium-iron hydrotalcite has the characteristics of no toxicity, no harm, no halogen and environmental protection.
Drawings
FIG. 1 is a scanning observation diagram of an SEM of example 3;
FIG. 2 is a scanning observation of BET in example 3;
FIG. 3 is a scanning observation of XRD of example 3;
fig. 4 is a scanning observation diagram of XPS of example 3;
fig. 5 is a graph showing kinetic models of adsorption of bromate in example 3 and comparative example 1.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are provided, but the protection scope of the present invention is not limited to the following embodiments.
The preparation process of intercalated magnesium-iron hydrotalcite with metaaluminate includes the following steps:
(1) Preparing a magnesium-iron mixed salt solution: adding magnesium salt and ferric salt into deionized water, and stirring to obtain magnesium-iron mixed salt solution; the molar ratio of magnesium to iron in magnesium salt to iron salt is (2-4): 1; the magnesium salt comprises magnesium chloride hexahydrate and the ferric salt comprises ferric nitrate nonahydrate;
(2) Preparing an aluminum-sodium mixed alkali solution: adding meta-aluminate and alkali into deionized water, and stirring to obtain aluminum-sodium mixed alkali solution; in meta-aluminate and alkali, the mole ratio of aluminum and hydroxyl is (0.5-2): 1; the meta-aluminate comprises sodium meta-aluminate, and the alkali comprises sodium hydroxide;
(3) Preparing a suspension: simultaneously dropwise adding a magnesium-iron mixed salt solution and an aluminum-sodium mixed alkali solution into deionized water, stirring, controlling the pH value of the solution to be 8-13, and continuing heating and stirring after the dropwise adding 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): 1, wherein, the temperature of heating and stirring is 80-90 ℃ for 1.5-2.5h; the stirring speed is 800-1200r/min;
(4) And (5) aging and crystallizing: standing the suspension, and then heating, aging and crystallizing to obtain a crystal precipitate; wherein the temperature of heating aging crystallization is 60-70 ℃ and the time is 20-24 hours;
(5) Filtering, washing and drying the crystal precipitate to obtain the metaaluminate intercalation magnesium-iron hydrotalcite. Wherein the temperature of the drying is 110-130 ℃ and the time is 1.5-2.5h.
Example 1
The preparation process of intercalated magnesium-iron hydrotalcite with metaaluminate radical includes 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, and after the mixture is stirred and dissolved completely, the mixture is kept stand for 10 minutes; 2g of sodium metaaluminate and 4g of sodium hydroxide are weighed, 200ml of deionized water is added, stirred and dissolved, and the mixture is kept stand for 10min.
(2) Preparing a suspension of a mixed acid solution and a mixed alkali solution: 100ml of deionized water was added to the beaker and stirred, the temperature was maintained at room temperature, and the prepared mixed acid solution and mixed alkali solution were added dropwise to the beaker at a constant speed, keeping the pH of the solution around 8. The volume ratio of the magnesium-iron mixed salt solution to the aluminum-sodium mixed alkali solution is about 0.5:1.
(3) And (5) aging and crystallizing: after the completion of the dropwise addition, the temperature was heated to 85℃and stirring was continued for 2 hours. After 2 hours, stirring is stopped, the temperature is controlled at 60 ℃, and the mixture is kept stand and aged for crystallization for 20 hours.
(4) Filtering, washing and drying: after aging and crystallization, filtering and precipitating by a vacuum pump, washing and precipitating to be neutral by deionized water, and then baking and precipitating by an oven at 120 ℃ for 2 hours to obtain the metaaluminate intercalation magnesian-iron hydrotalcite.
Example 2
The preparation process of intercalated magnesium-iron hydrotalcite with metaaluminate radical includes 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, and after the mixture is stirred and dissolved completely, the mixture is kept stand for 10 minutes; 4.1g of sodium metaaluminate and 5g of sodium hydroxide are weighed, 200ml of deionized water is added, stirred and dissolved, and the mixture is kept stand for 10min.
(2) Preparing a suspension of a mixed acid solution and a mixed alkali solution: 100ml of deionized water was added to the beaker and stirred, the temperature was maintained at room temperature, and the prepared mixed acid solution and mixed alkali solution were added dropwise to the beaker at a constant speed, keeping the pH of the solution around 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) And (5) aging and crystallizing: after the completion of the dropwise addition, the temperature was heated to 85℃and stirring was continued for 2 hours. After 2 hours, stirring is stopped, the temperature is controlled at 60 ℃, and the mixture is kept stand and aged and crystallized for 21 hours.
(4) Filtering, washing and drying: after aging and crystallization, filtering and precipitating by a vacuum pump, washing and precipitating to be neutral by deionized water, and then baking and precipitating by an oven at 120 ℃ for 2 hours to obtain the metaaluminate intercalation magnesian-iron hydrotalcite.
Example 3
The preparation process of intercalated magnesium-iron hydrotalcite with metaaluminate radical includes 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, and after the mixture is stirred and dissolved completely, the mixture is kept stand for 10 minutes; 6.1g of sodium metaaluminate and 8g of sodium hydroxide are weighed, 200ml of deionized water is added, stirred and dissolved, and the mixture is kept stand for 10min.
(2) Preparing a suspension of a mixed acid solution and a mixed alkali solution: 100ml of deionized water was added to the beaker and stirred, the temperature was maintained at room temperature, and the prepared mixed acid solution and mixed alkali solution were added dropwise to the beaker at a constant speed, keeping the pH of the solution around 10. The volume ratio of the magnesium-iron mixed salt solution to the aluminum-sodium mixed alkali solution is about 0.5:1.
(3) And (5) aging and crystallizing: after the completion of the dropwise addition, the temperature was heated to 85℃and stirring was continued for 2 hours. After 2 hours, stirring is stopped, the temperature is controlled at 60 ℃, and the mixture is kept stand and aged and crystallized for 22 hours.
(4) Filtering, washing and drying: after aging and crystallization, filtering and precipitating by a vacuum pump, washing and precipitating to be neutral by deionized water, and then baking and precipitating by an oven at 120 ℃ for 2 hours to obtain the metaaluminate intercalation magnesian-iron hydrotalcite.
The average pore diameter of the metaaluminate intercalation magnesium-iron 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 through electron microscope (SEM) scanning and pore diameter scanning (BET) observation, and the metaaluminate intercalation magnesium-iron hydrotalcite material is shown in figures 1-2; XRD scanning observation shows that the metaaluminate intercalation magnesium-iron hydrotalcite material prepared by the invention has characteristic peaks of (003), (006) and (009), accords with hydrotalcite structure, and is successfully intercalated by metaaluminate, as shown in figure 3; through XPS scanning observation, the meta-aluminate intercalation magnesium-iron hydrotalcite material prepared by the invention contains aluminum element, which shows that meta-aluminate is successfully intercalated therein, as shown in figure 4.
The prepared metaaluminate intercalated magnesium-iron hydrotalcite adopts metaaluminate intercalation, and after entering a water body, the metaaluminate can generate aluminum hydroxide in the water body due to ion exchange, and the aluminum hydroxide is a flocculating agent, has the effect of continuous water purification, is harmless to the human body, and does not cause secondary pollution to the water body.
Comparative example 1
The preparation method of the non-intercalated magnesium-iron 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, and after the mixture is stirred and dissolved completely, the mixture is kept stand for 10 minutes; 12.72g of sodium bicarbonate and 4.8g of sodium hydroxide are weighed, 500ml of deionized water is added, stirred and dissolved, and the mixture is kept stand for 10min.
(2) Preparing a suspension of a mixed acid solution and a mixed alkali solution: 100ml of deionized water was added to the beaker and stirred, the temperature was maintained at room temperature, and the prepared mixed acid solution and mixed alkali solution were added dropwise to the beaker at a constant speed, keeping the pH of the solution around 8.5. The volume ratio of the mixed salt solution to the mixed base solution is about 0.5:1.
(3) And (5) aging and crystallizing: after the completion of the dropwise addition, the temperature was heated to 85℃and stirring was continued for 2 hours. After 2 hours, stirring is stopped, the temperature is controlled at 60 ℃, and the mixture is kept stand and aged for crystallization for 23 hours.
(4) Filtering, washing and drying: 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 hydrotalcite.
As a result of adsorption of bromate, the equilibrium adsorption capacity of the metaaluminate 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. This shows that the metaaluminate intercalation 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-intercalation magnesium-iron hydrotalcite.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (1)
1. The application of the metaaluminate intercalation magnesium-iron hydrotalcite is characterized in that the hydrotalcite is applied to continuous water purification, and the preparation method of the hydrotalcite comprises the following steps:
(1) Preparing a mixed acid solution and a mixed alkali solution: weighing 12.857g magnesium chloride hexahydrate and 10g ferric nitrate nonahydrate, adding 100ml deionized water, stirring and dissolving completely, and standing for 10min; weighing 6.1g sodium metaaluminate and 8g sodium hydroxide, adding 200ml deionized water, stirring for dissolution, and standing for 10min;
(2) Preparing a suspension of a mixed acid solution and a mixed alkali solution: adding 100ml deionized water into a beaker, stirring, keeping the temperature at room temperature, dripping the prepared mixed acid solution and the mixed alkali solution into the beaker at a constant speed, keeping the pH of the solution to be 10, and keeping the volume ratio of the magnesium-iron mixed salt solution to the aluminum-sodium mixed alkali solution to be 0.5:1;
(3) And (5) aging and crystallizing: after the dripping is finished, heating the temperature to 85 ℃, continuing stirring for 2 hours, stopping stirring after 2 hours, controlling the temperature to 60 ℃, standing, and aging and crystallizing 22 h;
(4) Filtering, washing and drying: after aging and crystallization, filtering and precipitating by a vacuum pump, washing and precipitating to be neutral by deionized water, and then baking and precipitating 2h by an oven at 120 ℃ to obtain the meta-aluminate intercalated magnesium-iron hydrotalcite.
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