Preparation method of 1*1-type manganese oxide octahedral molecular sieves

A technology of pyrolusite and permanganate, applied in molecular sieve compounds, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve problems such as unfavorable practical application, high energy consumption, etc. The effect of high secondary yield and less pollution

Inactive Publication Date: 2012-10-17
INST OF URBAN ENVIRONMENT CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the high-temperature solid-phase method can generate a large amount of β-MnO 2 , but it consumes a lot of energy and is not conducive to practical application

Method used

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  • Preparation method of 1*1-type manganese oxide octahedral molecular sieves
  • Preparation method of 1*1-type manganese oxide octahedral molecular sieves
  • Preparation method of 1*1-type manganese oxide octahedral molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: adopt MnSO 4 As the divalent manganese source, take KMnO 4 Preparation of pyrolusite (β-MnO 2 ).

[0026] Weigh 2.8445 g KMnO 4 In a 1 L Erlenmeyer flask, add 450 mL deionized water to prepare a solution, and another 150 mL containing 0.24 mol MnSO 4 ·H 2 O and 15 mL of concentrated HNO 3 The mixed solution of KMnO was added directly 4 The solution was placed in a collector-type constant temperature heating magnetic stirrer at 100°C for reflux reaction for 36 hours, taken out and cooled naturally, then filtered, and the reaction product was washed with deionized water until the conductivity of the filtrate was less than 30 uS / cm. The product was dried in an oven at 60 °C, and its crystal structure was characterized by XRD ( figure 1 ), FTIR analysis of its main functional groups ( figure 2 ), scanning electron microscopy to characterize its morphology ( image 3 ), TEM morphology ( Figure 4 ) and the electron diffraction structure diagram ( F...

Embodiment 2

[0029] Embodiment 2: with Mn (NO 3 ) 2 Synthesis of pyrolusite (β-MnO 2 ).

[0030] Weigh 2.8445 g KMnO 4 In a 1 L Erlenmeyer flask, add 450 mL deionized water to prepare a solution, and 150 mL containing 0.24 mol Mn(NO 3 ) 2 and 15 mL concentrated HNO 3 The mixed solution of KMnO was added directly 4 Solution, placed in a collector-type constant temperature heating magnetic stirrer at 100 ° C for 36 hours of reflux reaction, taken out and filtered after natural cooling, the reaction product was washed with deionized water until the conductivity of the filtrate was less than 30 uS / cm to obtain β-MnO 2 Nano stave.

[0031]

Embodiment 3

[0032] Embodiment 3: with MnCl 2 Synthesis of pyrolusite (β-MnO 2 ).

[0033] Weigh 2.8445 g KMnO4 In a 1 L Erlenmeyer flask, add 450 mL deionized water to prepare a solution, and 150 mL containing 0.24 mol MnCl 2 and 15 mL concentrated HNO 3 The mixed solution of KMnO was added directly 4 Solution, placed in a collector-type constant temperature heating magnetic stirrer at 100 ° C for 36 hours of reflux reaction, taken out and filtered after natural cooling, the reaction product was washed with deionized water until the conductivity of the filtrate was less than 30 uS / cm to obtain β-MnO 2 Nano stave.

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Abstract

The invention discloses a preparation method of 1*1-type manganese oxide octahedral molecular sieve (pyrolusite, beta-MnO2) nano-rods, and especially relates to a preparation method which is used for synthesizing single-phase 1*1-type manganese oxide octahedral molecular sieve nano-rods having good crystallinity under the conditions of non-pressurized heating reflux so that a large amount of the 1*1-type manganese oxide octahedral molecular sieve nano-rods are synthesized by one step. The preparation method provided by the invention is characterized in that a mixed solution containing one or more salts of single divalent manganese, permanganates and strong acids undergoes a reflux reaction to produce the 1*1-type manganese oxide octahedral molecular sieve nano-rods under the control of a concentration, a temperature and time. The preparation method allows mild reaction conditions, can be operated simply, can be controlled easily, has low energy consumption, produces low pollution and has a high single yield. The 1*1-type manganese oxide octahedral molecular sieve nano-rods obtained by the preparation method can be used for catalysts, magnetic materials and chemical power source materials.

Description

technical field [0001] The present invention relates to 1×1 manganese oxide octahedral molecular sieve (pyrolulusite or β-MnO 2 ) method of preparation. The present invention is particularly suitable for synthesizing well-crystallized single-phase 1×1 manganese-oxygen octahedral molecular sieves (β-MnO 2 ), so that a large amount of 1 × 1 manganese oxide octahedral molecular sieves can be synthesized at one time under simple conditions, which belongs to the inorganic preparation method of manganese oxide nano functional materials. [0002] Background technique [0003] Nano-manganese oxide octahedral molecular sieves have rich structural chemical characteristics and excellent physical and chemical properties, and show good application prospects in modern industry and environmental fields, and are one of the hotspots in the international research on nano-functional materials. β-MnO 2 With the advantages of stable structure and high chemical activity, as a nano-functional ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/02C01B39/00C01B37/00
Inventor 崔浩杰付明来李丽
Owner INST OF URBAN ENVIRONMENT CHINESE ACAD OF SCI
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