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Crystalline catalysis material for reaction of preparing dimethyl ether from methanol by dehydration and preparation method thereof

A catalytic material, methanol dehydration technology, applied in the field of chemical materials, can solve the problems of high molecular sieve cost, high reaction temperature, non-uniform active points, etc., and achieve the effect of high catalytic active point density, reduced reaction cost, and high water resistance.

Inactive Publication Date: 2010-10-27
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

γ-Al 2 o 3 , molecular sieve, and aluminum phosphate can be used as catalysts for this reaction, but they have their own disadvantages: the surface of aluminum phosphate is prone to carbon deposition and deactivation, the cost of molecular sieve is high, and γ-Al 2 o 3 The reaction temperature is high, so its use is limited
But commonly used porous materials, such as: γ-Al 2 o 3 , activated carbon, ion exchange resin, etc. are considered to be a class of materials with "unclear" composition and structure. It is difficult to clarify the microstructure of the catalyst by using them as carriers to carry polyacids.
In addition, these supported catalysts also have disadvantages such as low loading capacity, agglomeration of active sites, and uneven active sites.

Method used

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  • Crystalline catalysis material for reaction of preparing dimethyl ether from methanol by dehydration and preparation method thereof
  • Crystalline catalysis material for reaction of preparing dimethyl ether from methanol by dehydration and preparation method thereof
  • Crystalline catalysis material for reaction of preparing dimethyl ether from methanol by dehydration and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: [Cu 2 (BTC) 4 / 3 ] 6 [H 4 SiW 12 o 40 ] preparation

[0026] H was prepared according to the literature method 4 SiW 12 o 40 ·xH 2 O. (North, E.O.Inorg.Synth.1939, 1, 129.) H 4 SiW 12 o 40 ·xH 2 O, Trimellitic acid, copper sulfate, tetramethylammonium chloride and water are mixed at a material ratio of 1:5:10:8:2000, stirred, and the pH of the mixture is adjusted to 0.5, under hydrothermal autogenous pressure conditions Under 120 degrees Celsius, crystals were obtained after 8 hours. The crystals were collected, refluxed in ethanol, and heated to 160°C under vacuum, and the target crystalline material was obtained after 2 hours.

Embodiment 2

[0027] Example 2: [Cu2 (BTC) 4 / 3 ] 6 [H 4 GeW 12 o 40 ] preparation

[0028] H was prepared according to the literature method 4 GeW 12 o 40 14H 2 O. (Rocchiccioli-Deltcheff et al.Inorg.Chem.1983, 22, 207-216) H 4 GeW 12 o 40 14H 2 O, Trimellitic acid, copper chloride, tetraethylammonium chloride and water are mixed at a material ratio of 1: 22: 30: 25: 24000, stirred, and the pH of the mixture is adjusted to 2.5. Under the condition of 240 degrees Celsius, crystals were obtained after 48 hours. The crystals were collected, refluxed in ethanol, and heated to 240°C under vacuum, and the target crystalline material was obtained after 12 hours.

Embodiment 3

[0029] Embodiment 3: [Cu 2 (BTC) 4 / 3 ] 6 [H 3 PMo 12 o 40 ] preparation

[0030] H was prepared according to the literature method 3 PMo 12 o 40 14H 2 O. (Rocchiccioli-Deltcheff et al.Inorg.Chem.1983, 22, 207-216) H 3 PMo 12 o 40 14H 2 O, Trimellitic acid, copper nitrate, ammonium chloride and water are mixed at a material ratio of 1:5:10:8:2000, stirred, and the pH of the mixture is adjusted to 0.5. Under hydrothermal autogenous pressure conditions, 120 degrees Celsius, crystals were obtained after 8 hours. The crystals were collected, refluxed in ethanol, and heated to 160°C under vacuum, and the target crystalline material was obtained after 2 hours.

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Abstract

The invention belongs to the technical field of chemical materials and relates to a crystalline catalysis material for reaction of preparing dimethyl ether from methanol by dehydration and a preparation method thereof. In the crystalline catalysis material, a porous metal organic frame constructed by copper and trimesic acid is taken as a carrier to support Keggin type polyoxometallate. The method for preparing the crystalline catalysis material comprises the steps of: mixing the Keggin type polyoxometallate, trimesic acid, copper salt, ammonium salt and water in a certain molar ratio, and obtaining a crystal under the hydrothermal self-generated pressure; performing reflux on the obtained crystal in alcohol or performing ion exchange on the obtained crystal in aqueous solution of acid, and performing heat treatment on the crystal under the vacuum condition to obtain the material. The crystalline catalysis material has the advantages of low reaction temperature, high water resistance, simple preparation method, low cost, no corrosion or pollution, and suitability for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical materials, and in particular relates to a kind of crystalline catalytic material which takes a porous metal-organic framework constructed by copper and trimesic acid as a carrier and supports Keggin type polyoxometalates and a preparation method thereof. Background technique [0002] Dimethyl ether (DME) is an important "green chemical" raw material and a potential clean energy. Studies have shown that engines using dimethyl ether instead of diesel can obtain higher specific power and thermal efficiency, and have the advantages of low noise and ultra-low emissions, and can meet Euro III and California Ultra Emissions (ULEV) standards. The development and application of dimethyl ether has huge social, economic and strategic significance. [0003] The production method of dimethyl ether is mainly based on methanol as raw material, and it is obtained after dehydration under the action of a catalyst...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C43/04C07C41/09
Inventor 刘术侠梁大栋
Owner NORTHEAST NORMAL UNIVERSITY
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