Preparation method of a mesoporous hollow nitrogen-doped carbon-coated copper nanocatalyst

A nano-catalyst, hollow technology, applied in catalyst activation/preparation, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of hindering the entry and exit of reactants, restricting catalytic activity, etc. The effect of good stability

CN106563484BActive Publication Date: 2019-01-22TAIYUAN UNIV OF TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2019-01-22

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Abstract

The invention belongs to the field of carbon-based composite material preparation. Specifically, it is a preparation method of mesoporous hollow nitrogen-doped carbon-coated copper nanocatalyst, using polypyrrole as the carbon source and nitrogen source, copper sulfate as the active component precursor, and PS micro-catalyst. The ball is used as a template, and under the appropriate surfactant, it is sequentially wrapped in multiple layers and then carbonized at high temperature. After activation, a mesoporous nitrogen-doped carbon-coated copper catalyst with controllable morphology and size is obtained, which is reflected in the reaction of preparing DMC from methanol. Higher catalytic activity and better stability. The prepared catalyst has a significant effect in avoiding the agglomeration and stripping of active components and improving the reaction catalytic activity. The experimental data is accurate and detailed, the cost is low, and the raw materials are easily available. The product is a black powder with a particle diameter of less than 400 nm. The purity of the product reaches 98.9%. The DMC space-time yield in the reaction can reach 1251 mg / g∙h, and the selectivity is as high as 99.99%.
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Description

technical field

[0001] The invention belongs to the field of carbon-based composite material preparation, in particular to a method for preparing a mesoporous hollow nitrogen-doped carbon-coated copper nano-catalyst, which can be used to catalyze the oxidative carbonylation of methanol to prepare dimethyl carbonate. Background technique

[0002] Dimethyl carbonate (DMC) is a downstream product of methanol and has a wide range of uses. Compared with various preparation methods, methanol oxidative carbonylation method has become a research hotspot in recent years because of its low production cost, high selectivity, and low corrosion to equipment.

[0003] In the catalyst research of methanol oxidative carbonylation reaction, we proposed a composite material of hollow carbon spheres coated with copper nanoparticles. On the one hand, the barrier effect of the carbon layer is used to limit the agglomeration of active components. specific microenvironment.

[0004] Copper nanoc...

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Embodiment Construction

[0019] The chemical material used in the present invention is: deionized water, ammonia water, copper sulfate, cetyltrimethylammonium bromide (CTAB), polyvinylpyrrolidone (PVP), pyrrole, styrene, azobisisobutyronitrile (AIBN), potassium persulfate, hydrazine hydrate, high-purity nitrogen, high-purity hydrogen, the preparation dosage is as follows: in grams, milliliters, centimeters 3 as a unit of measurement

[0020] Deionized water: H 2 O Liquid 3000ml±50ml

[0021] Ammonia:NH 3 •H 2 O Liquid 6 ml±0.1 ml

[0022] Pyrrole: C 4 h 5 N liquid 3 ml±0.1 ml

[0023] Styrene:C 8 h 8 Liquid 9ml±0.1ml

[0024] Hydrazine hydrate: H 6 N 2 O Liquid 280 µl±0.1 µl

[0025] Azobisisobutyronitrile: C 8 h 12 N 4 Solid 1 g±0.001 g

[0026] Potassium persulfate: K 2 S 2 o 8 Solid 1 g±0.001 g

[0027] Copper Sulfate: CuSO 4 • 5H 2 O solid 2 g±0.001 g

[0028] Hexadecyltrimethylammonium bromide: C1 9 h 42 BrN solid 1 g±0.001 g

[0029] Polyvinylpyrrolidone: (C 6 h 9...