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Catalyst for preparing dimethyl carbonate from methanol, carbon dioxide and 2-cyanopyridine and its preparation method and application

A technology of dimethyl carbonate and cyanopyridine, which is applied in the field of preparation of dimethyl carbonate, can solve the problems of difficult separation and purification of products, low recycling efficiency, consumption of dehydrating agent, etc., to facilitate large-scale production, increase production capacity, and reduce costs low effect

Active Publication Date: 2022-03-11
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2013, it was reported that the use of 2-cyanopyridine as a high-efficiency dehydrating agent achieved a near-stoichiometric conversion reaction of methanol. At the same time, the dehydrating agent can also be used for catalytic recycling (ChemSusChem 2013, 6, 1341), but the efficiency of recycling is very low
On the one hand, the by-product generation process consumes dehydrating agent, which increases the cost; on the other hand, the by-product brings difficulties to the separation and purification of products, and the process is more complicated, which greatly increases energy consumption

Method used

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  • Catalyst for preparing dimethyl carbonate from methanol, carbon dioxide and 2-cyanopyridine and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Prepare the concentration of Cr ion to be 0.1 g·mL -1 6 mL of chromium nitrate solution, and γ-Al with a particle size of 20 nm was added to the solution 2 o 3 The solid was 8.9 g, and stirred evenly, then 10 mL of H3BO3 solution with a concentration of 0.9 mol / L was added, stirred again to mix evenly, soaked for 6 h, then dried at 100 °C for 12 h, and the obtained solid was ground, 400 °C Calcined under the same conditions for 6 h to obtain the catalyst. Take 10 g of catalyst raw powder and fill it into the tank reactor. Methanol and 2-cyanopyridine are mixed and miscible at a molar ratio of 3:1 and then fed in liquid form. The liquid material accounts for 12% of the reactor volume. CO2 is fed in a gaseous state, and CO2 is charged to 1 MPa. The reaction temperature was 100 °C, the mass ratio of catalyst to methanol was 0.06, the residence time of the reactants in the reaction bed was 8 h, the conversion rate of methanol was 88.7%, the selectivity of DMC was 100%, a...

Embodiment 2

[0030] Prepare Zr ion concentration to be 0.07 g·mL -1 10 mL of zirconium nitrate solution, and SiO with a particle size of 20 nm was added to the solution 2 Solid 8.95 g, and stir evenly, then add the H that concentration is 0.45 mol / L 3 BO 3 10 mL of the solution was stirred and mixed evenly, impregnated for 6 h, then dried at 100 °C for 16 h, the obtained solid was ground, and calcined at 400 °C for 10 h to obtain the catalyst. Take 10 g of catalyst raw powder and fill it into the tank reactor. Methanol and 2-cyanopyridine are mixed and miscible at a molar ratio of 1:1 and then fed in liquid form. The liquid material accounts for 25% of the reactor volume. CO2 is fed in a gaseous state, and CO2 is charged to 5 MPa. The reaction temperature was 120 °C, the mass ratio of catalyst to methanol was 0.05, the residence time of the reactants in the reaction bed was 8 h, the methanol conversion rate was 91.2%, the DMC selectivity was 100%, and the number of catalyst cycles was ...

Embodiment 3

[0032] Prepare the concentration of Mn ion to be 0.15 g·mL -1 10 mL of manganese nitrate solution, the concentration of Ni ions is 0.08 g·mL -1 10 mL of nickel nitrate solution, and γ-Al with a particle size of 50 nm was added to the mixed solution 2 o 3 Solid 16.6 g, and stir evenly, then add the H that concentration is 0.7 mol / L 3 20 mL of PO4 solution was stirred and mixed evenly again, impregnated for 8 h, then dried at 120 °C for 8 h, the obtained solid was ground, and calcined at 500 °C for 4 h to obtain the catalyst. Take 10 g of catalyst raw powder and fill it into the tank reactor. Methanol and 2-cyanopyridine are mixed and miscible at a molar ratio of 1:2 and then fed in liquid form. The liquid material accounts for 25% of the reactor volume, and the CO 2 Feed in gaseous state, filled with CO 2to 3 MPa, the reaction temperature is 115°C, the mass ratio of catalyst to methanol is 0.1, the residence time of the reactants in the reactor is 6 h, the methanol convers...

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Abstract

The invention relates to the field of preparation of dimethyl carbonate, and a catalyst for preparing dimethyl carbonate from methanol, carbon dioxide and 2-cyanopyridine, comprising metal oxides, additives and carriers, and the metal oxides are 0.5-20% by weight. %, additives are 0.5~2%, and the rest are carriers. The present invention also relates to the preparation method and application of the catalyst. The catalyst preparation process of the invention does not use any organic solvent and precious metal, has low cost and is easy to produce on a large scale.

Description

technical field [0001] The invention relates to the field of preparing dimethyl carbonate from methanol, carbon dioxide and 2-cyanopyridine. Background technique [0002] carbon dioxide (CO 2 ) is an environmentally friendly renewable carbon-feedstock that can be applied to the preparation of many kinds of compounds and clean fuels. Dimethyl carbonate is a green chemical with broad uses and markets. The ideal synthetic route is methanol and CO 2 reaction, the by-product is water. China is rich in coal resources. With the development of coal chemical industry, CO 2 Emissions are inevitable. In addition, coal-based methanol production technology is mature, and methanol and CO 2 Synthesizing dimethyl carbonate as a raw material can not only broaden the utilization channels of methanol, but also effectively realize CO 2 high value utilization. The industrialization of this route will expand and promote the development of clean utilization of coal to prepare chemicals. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/26B01J21/08B01J27/16B01J23/80B01J23/86B01J23/755B01J23/10B01J23/889B01J37/02B01J37/08C07C68/04C07C69/96
CPCB01J23/26B01J21/08B01J27/16B01J23/80B01J23/862B01J23/755B01J23/10B01J23/8892B01J23/002B01J37/0201B01J37/088B01J37/082C07C68/04B01J2523/00B01J35/23C07C69/96B01J2523/305B01J2523/31B01J2523/67B01J2523/41B01J2523/48B01J2523/51B01J2523/72B01J2523/847B01J2523/15B01J2523/3706B01J2523/27B01J2523/842B01J2523/845Y02P20/141
Inventor 宋清文刘平张侃张乾霞韩丽华荀家瑶刘增厚
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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