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A preparation method of three-dimensional porous graphene-supported nano-magnesium-aluminum hydrotalcite defluoridation agent

A three-dimensional porous and graphene technology, applied in chemical instruments and methods, water/sewage treatment, adsorption water/sewage treatment, etc., can solve the problems of poor controllability, uneven particle size, high local concentration, etc., and achieve enhanced adsorption treatment effect, reduction of reaction rate, effect of nanoparticle uniformity

Active Publication Date: 2015-11-25
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, at present, nano-magnesium aluminum hydrotalcite mainly adopts the co-precipitation method of salt solution and alkali solution. Since the reaction is carried out in the same phase and the reaction rate is fast, the local concentration is too high, the controllability is poor, and the formed particles are often uneven in size, which is easy to Agglomeration and coagulation occur, and the specific surface area decreases, the dispersion is poor, and the effect of fluorine adsorption treatment is not good

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step 1: first anneal the graphite powder at 200°C for 2 hours, and then oxidize it to obtain graphene oxide ( Chem.Commun., 2011, 47, 10389). Weigh 1g of graphene oxide and add it to a 250mL three-necked round-bottomed flask, then add 50mL of 2% oxalic acid solution, stir for 2 hours at 85°C, filter, wash, and freeze-dry at -70°C for 20 hours to obtain the required 3D porous graphene.

[0026] Step 2: Prepare 200mL of a mixed solution of magnesium chloride and aluminum chloride in a 500mL beaker, wherein the concentrations of magnesium chloride and aluminum chloride are 2% and 0.5% respectively, and then soak 1g of three-dimensional porous graphene in it. After 6 hours, Filter and dry to obtain three-dimensional porous graphene loaded with magnesium and aluminum ions.

[0027] Step 3: Put 1 g of three-dimensional porous graphene loaded with magnesium and aluminum ions into a 500 mL beaker, quickly add 200 mL of 0.1% ammonium bicarbonate solution, stir rapidly and heat...

Embodiment 2

[0030] Step 1: first anneal the graphite powder at 300°C for 3 hours, and then oxidize it to obtain graphene oxide (same as Example 1). Weigh 2g of graphene oxide and add it to a 250mL three-necked round-bottomed flask, then add 120mL of 2% oxalic acid solution, stir for 2 hours at 60°C, filter, wash, and freeze-dry at -60°C for 48 hours to obtain the required 3D porous graphene.

[0031] Step 2: Prepare 300mL of a mixed solution of magnesium nitrate and aluminum sulfate in a 1000mL beaker, so that the concentrations of magnesium nitrate and aluminum sulfate are 1.5% and 0.5% respectively, then soak 2g of three-dimensional porous graphene in it, and filter after 10 hours After drying, three-dimensional porous graphene loaded with magnesium and aluminum ions is obtained.

[0032] Step 3: Put 2g of three-dimensional porous graphene loaded with magnesium and aluminum ions into a 1000mL beaker, add 400mL of 0.4% ammonium bicarbonate solution, stir rapidly and heat up to 80°C, rea...

Embodiment 3

[0035] Step 1: first anneal the graphite powder at 280°C for 3 hours, and then oxidize it to obtain graphene oxide (same as Example 1). Weigh 5g of graphene oxide and add it to a 500mL three-necked round-bottomed flask, then add 300mL of 2% oxalic acid solution, stir for 2 hours at 70°C, filter, wash, and freeze-dry at -20°C for 48 hours to obtain the required 3D porous graphene.

[0036]Step 2: Prepare 300mL of a mixed solution of magnesium chloride and aluminum sulfate in a 1000mL beaker so that the concentrations of magnesium chloride and aluminum sulfate are 3% and 1% respectively, then soak 5g of three-dimensional porous graphene in it, and filter and dry after 8 hours. Three-dimensional porous graphene loaded with magnesium and aluminum ions was obtained.

[0037] Step 3: Put 5g of three-dimensional porous graphene loaded with magnesium and aluminum ions into a 1000mL beaker, quickly add 400mL of 0.5% sodium bicarbonate solution, stir rapidly and heat up to 70°C, react ...

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Abstract

The invention discloses a preparation method of a three-dimensional porous graphene-loaded nanometer magnesium-aluminum hydrotalcite fluorine removal agent. The preparation method comprises the following steps: (a) preparing the three-dimensional porous graphene; (b) preparing magnesium-aluminum solution, immersing the three-dimensional porous graphene in the solution; and (c) separating the immersed three-dimensional porous graphene, drying in a vacuum condition, adding into a carbon source weak base dilute solution, reacting, standing, aging, filtering, washing, and drying, so as to obtain the three-dimensional porous graphene-loaded nanometer magnesium-aluminum hydrotalcite fluorine removal agent. Due to the adoption of the method, the agglomeration characteristic of the magnesium-aluminum hydrotalcite prepared by a traditional method is overcome, the specific surface area of the nanometer magnesium-aluminum hydrotalcite is improved; meanwhile, because the carboxylic groups in the three-dimensional porous graphene are combined with the magnesium-aluminum atoms, the nanometer particles can be effectively limited into a porous channel of the three-dimensional porous graphene, losing of the nanometer material is avoided in a using process, and the material has a significant effect in fluorine-containing water treatment.

Description

technical field [0001] The present invention relates to a method for preparing a three-dimensional porous graphene-loaded nano-magnesium-aluminum hydrotalcite defluoride agent, in particular, it relates to a preparation method for loading a nano-magnesium-aluminum hydrotalcite in a three-dimensional porous graphene substrate, and the obtained material can realize The invention relates to the effective removal of fluorine ions in water, belonging to the technical field of environmental treatment. Background technique [0002] Fluorine is a trace element of life closely related to human health, mainly distributed in the bones and teeth of the human body. Fluoride exists widely in water bodies in nature, and the existence of a moderate amount of fluorine in water is beneficial to human health. However, excessive fluorine intake will lead to poisoning of human beings, animals and plants. It has been reported that when the fluoride ion concentration in water is 2mg / L, obvious d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30C02F1/28C02F1/58
Inventor 孔令涛孙柏张开胜王进罗涛贾勇金震刘锦淮
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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