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Preparation method of graphene-supported nano MnOOH composite material

A composite material and graphene technology, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve problems such as prone to agglomeration and affect the excellent performance of nano-effects, and achieve convenient and excellent post-processing Catalytic performance, effect of low reaction temperature

Active Publication Date: 2012-12-19
TECH TRANSFER CENT CO LTD NANJING UNIV OF SCI & TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the MnOOH nanomaterials prepared by the prior art are prone to agglomeration during the application process, which seriously affects the excellent performance due to the nano-effect.

Method used

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  • Preparation method of graphene-supported nano MnOOH composite material
  • Preparation method of graphene-supported nano MnOOH composite material
  • Preparation method of graphene-supported nano MnOOH composite material

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Experimental program
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Effect test

preparation example Construction

[0018] to combine figure 1 , the preparation method of graphene-loaded nano-MnOOH composite material of the present invention, comprises the following steps:

[0019] Step 1: MnCl 2 4H 2 O. Graphite oxide and isopropanol are mixed to make a solution, and dispersed evenly by ultrasonic;

[0020] Step 2: KMnO 4 Add water and water to the solution prepared in step 1, stir evenly, the concentration of graphite oxide in isopropanol is 0.00111~0.0222g / mL, MnCl 2 4H 2 The concentration of O in isopropanol is 0.0018~0.054g / mL, MnCl 2 4H 2 O and KMnO 4 The mass ratio of KMnO is 1.42~2.50:1, KMnO 4 The concentration in water is 0.0127~0.15g / mL;

[0021] Step 3: React the mixed solution in step 2 at a constant temperature under sealed conditions for a period of time to obtain a black precipitate. The reaction equation is: 2KMnO 4 +3MnCl 2 +2H 2 O→5MnO 2 +2KCl+4HCl, the reaction time is 30min~24h, and the reaction temperature is 90~150℃;

[0022] Step 4: Centrifuge and wash...

Embodiment 1

[0027] Step 1: 0.36g MnCl 2 4H 2 O. Mix 0.0665g graphite oxide with 30mL isopropanol to form a solution, and disperse evenly by ultrasonic;

[0028] Step 2: Add 0.20g KMnO 4 Add 5mL of water to the solution prepared in step 1, and stir evenly;

[0029] Step 3: React the mixture in step 2 at 120°C for 12 hours under sealed conditions to obtain a black precipitate. The reaction equation is: 2KMnO 4 +3MnCl 2 +2H 2 O→5MnO 2 +2KCl+4HCl;

[0030] Step 4: centrifuge and wash the black precipitate obtained from the reaction, add it to 30mL ethylene glycol, and stir evenly;

[0031] Step 5: React the mixture in step 4 at 120°C for 16 hours under sealed condition, the reaction equation is: 2MnO 2 +HOCH 2 -CH 2 OH→2MnOOH+HOCH 2 -CHO;

[0032] Step 6: Centrifuge, wash, dry, and grind the product obtained from the reaction in step 5 to obtain a graphene-loaded nano-MnOOH composite material. Its XRD test result is as follows figure 2 As shown in (a), the transmission electron...

Embodiment 2

[0035] Step 1: 0.054g MnCl 2 4H 2 O. 0.0399g of graphite oxide was mixed with 30mL of isopropanol to form a solution, which was uniformly dispersed by ultrasonic;

[0036] Step 2: Add 0.038g KMnO 4 Add 3mL water to the solution prepared in step 1, and stir evenly;

[0037] Step 3: React the mixture in step 2 at 120°C for 12 hours under sealed conditions to obtain a black precipitate. The reaction equation is: 2KMnO 4 +3MnCl 2 +2H 2 O→5MnO 2 +2KCl+4HCl;

[0038] Step 4: Centrifuge and wash the black precipitate obtained from the reaction, add it to 12 mL of ethylene glycol, and stir evenly;

[0039] Step 5: React the mixture in step 4 at 120°C for 16 hours under sealed condition, the reaction equation is: 2MnO 2 +HOCH 2 -CH 2 OH→2MnOOH+HOCH 2 -CHO;

[0040] Step 6: Centrifuge, wash, dry, and grind the product obtained from the reaction in step 5 to obtain a graphene-loaded nano-MnOOH composite material.

[0041] After adding 2wt% of the obtained graphene-MnOOH comp...

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Abstract

The invention relates to a preparation method of a graphene-supported nano MnOOH composite material, which comprises the following steps: I, mixing and preparing MnCl2.4H2O, graphite oxide and isopropanol into a solution which is uniformly diffused under ultrasound; II, adding KMnO4 and water into the solution prepared in the step I, and stirring uniformly; III, performing a constant-temperature reaction on the mixed solution in the step II in a sealed condition for a certain period of time to obtain black precipitates; IV, centrifuging and washing the black precipitates obtained by the reaction, adding the product into glycol and stirring uniformly; V, performing a constant-temperature reaction on the mixed solution in the step IV in a sealed condition; and VI, centrifuging, washing, drying and grinding the product obtained by the reaction in the step V to obtain the graphene-supported nano MnOOH composite material. The preparation method provided by the invention is a soft chemical method easy to operate, and can prepare the graphene-supported nano MnOOH composite material with excellent catalytic performance under mild conditions.

Description

technical field [0001] The invention relates to a method for preparing a nanocomposite material, in particular to a method for preparing graphene-loaded nano MnOOH. Background technique [0002] MnOOH is a widely studied multifunctional transition metal perhydroxide, which is widely used in catalysis, molecular absorption, system simulation and other fields, and is an important precursor of lithium-ion batteries. However, the MnOOH nanomaterials prepared by the prior art are prone to agglomeration during the application process, which seriously affects the excellent performance due to the nano-effect. Further improving the dispersion and performance of nano-MnOOH is an urgent problem to be solved. [0003] Graphene is a two-dimensional crystal composed of a single layer of carbon atoms arranged in a honeycomb shape. It has attracted much attention due to its large specific surface area, excellent electrical conductivity and unique physical and chemical properties. There ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/34B01J37/34H01M4/90
CPCY02E60/50
Inventor 汪信朱俊武陈胜刘孝恒韩巧凤杨绪杰陆路德
Owner TECH TRANSFER CENT CO LTD NANJING UNIV OF SCI & TECH
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