Preparation of organic/inorganic nano media pores hybridization catalyst utilized for synthesizing methyl carbonate as well as its application

A technology of dimethyl carbonate and inorganic nanometers, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, carbonate/haloformate preparation, etc., can solve the problem of equipment corrosion, Poor solubility, low reaction efficiency and other problems, to achieve the effect of improving catalytic efficiency and reducing acidity

Inactive Publication Date: 2003-10-08
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, cuprous chloride (CuCl) is highly corrosive to the reaction device, and anti-corrosion materials such as glass or enamel lining must be added to the inner wall of the reactor, making it difficult to realize a large-scale device.
In addition, due to the extremely poor solubility of CuCl in the reaction system, a high concentration of CuCl must be used in the Eni Chem process to obtain a sufficient reaction rate
Chinese patent CN1197792A (1998) uses CuCl as the main catalyst, magnesium chloride, calcium chloride, etc. as auxiliary agents to prepare a composite catalyst modified by alkaline earth metal salts, which improves the solubility of cuprous chloride in the reaction solution to a certain extent. Improves catalyst activity, but does not solve the problem of corrosion to equipment
Chinese patent CN1333086A (2002) has announced to take CuCl as main catalyst, and the composite catalyst that nitrogen-containing heterocyclic compound ...

Method used

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  • Preparation of organic/inorganic nano media pores hybridization catalyst utilized for synthesizing methyl carbonate as well as its application
  • Preparation of organic/inorganic nano media pores hybridization catalyst utilized for synthesizing methyl carbonate as well as its application
  • Preparation of organic/inorganic nano media pores hybridization catalyst utilized for synthesizing methyl carbonate as well as its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 10g of MCM-41 sample that has been pretreated for 10 hours at 200°C into 100mL of freshly steamed toluene, stir well, then add 40mL (EtO) 3 Si(CH 2 ) 3 NH2 and 50mL of anhydrous ethyl formate, heated to 120°C, continuously stirred and refluxed for 12h, washed with absolute ethanol several times, filtered with suction, and dried in a vacuum oven; the above product was added to 100mL of ethanol, Then add 3g CuCl 2 , stirred and refluxed for 10h, washed the reaction product several times with absolute ethanol, and dried in vacuum to obtain 12g CuCl 2 -amide-MCM-41 nano mesoporous hybrid catalyst (Cu content: 3wt%).

[0016] In a 500ml autoclave, add 100ml methanol, 8g CuCl 2 -amide-MCM-41 nanometer mesoporous hybrid catalyst, with mixed gas (O 2 : 8%, CO: 92%) to replace the air in the reactor, and then use this gas to pressurize to 3.0MPa at room temperature. The reaction was carried out at 120° C. for 3 hours. After cooling, it was analyzed by gas chromatograp...

Embodiment 2

[0018] Add 4g of MCM-41 sample pretreated at 200°C for 10h into 100mL of freshly distilled toluene, stir well, then add 40mL (EtO) 3 Si(CH 2 ) 3 NHCH 2 CH 2 NH 2 and 50mL of anhydrous ethyl formate, heated to 120°C, continuously stirred and refluxed for 12h, washed with absolute ethanol several times, filtered with suction, and dried in a vacuum oven; the above product was added to 100mL of ethanol, Then add 3g CuCl 2 , stirred and refluxed for 10h, washed the reaction product several times with absolute ethanol, and dried in vacuum to obtain 12g CuCl 2 - diamide-MCM-41 nano-mesoporous hybrid catalyst (Cu content: 10 wt%).

[0019] In a 500ml autoclave, add 100ml methanol, 8g CuCl 2 -diamide-MCM-41 nanometer mesoporous hybrid catalyst, with mixed gas (O 2 : 8%, CO: 92%) to replace the air in the reactor, and then use this gas to pressurize to 3.0MPa at room temperature. The reaction was carried out at 120° C. for 3 hours. After cooling, it was analyzed by gas chromat...

Embodiment 3

[0023] Add 10g of HMS sample after 10h pretreatment at 200℃ into 100mL of freshly distilled toluene, stir well, add 40mL (EtO) 3 Si(CH 2 ) 3 NHCH 2 CH 2 NH 2 and 50mL of anhydrous ethyl formate, heated to 120°C, continuously stirred and refluxed for 12h, washed with absolute ethanol several times, filtered with suction, and dried in a vacuum oven; the above product was added to 100mL of ethanol, Then add 5g CuCl, stir and reflux for 10h, wash the reaction product several times with absolute ethanol, and vacuum dry to obtain 12g CuCl-diamide-HMS nano-mesoporous hybrid catalyst (Cu content: 4wt%).

[0024] In 500ml autoclave, add 100ml methyl alcohol, 8g CuCl-diamide-HMS nano mesoporous hybrid catalyst, with mixed gas (O 2 : 8%, CO: 92%) to replace the air in the reactor, and then use this gas to pressurize to 3.0MPa at room temperature. The reaction was carried out at 120° C. for 4 hours. After cooling, it was analyzed by gas chromatography. The selectivity of dimethyl ...

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Abstract

A nano-class organic/inorganic mesoporous hybridizing catalyst for preparing dimethyl carbonate by liquid-phase oxidization and carbonylation of methanol contains copper halides and the carrier whichis a nano-class organic/inorganic mesoporous hybridizing material with specially treated surface for effectively dispersing the copper halides on it. The said dimethyl carbonate is prepared from methanol, catalyst, CO and O2 through reaction at 110-140 deg.C and 2.0-5.0 MPa. Its advantages are high selectivity, activity and stability, low corrosion and cyclic use of catalyst.

Description

technical field [0001] The invention belongs to the preparation and use method of an organic / inorganic nanometer mesoporous hybrid composite catalyst used for methanol liquid-phase oxidative carbonylation to synthesize dimethyl carbonate. Background technique [0002] As a new type of organic chemical raw material with high added value, the synthesis and application of dimethyl carbonate (DMC) has attracted widespread attention in recent years. Dimethyl carbonate is known as a "green" chemical product and a "new building block" for chemical synthesis. Because of its high activity, it can replace highly toxic and carcinogenic phosgene, dimethyl sulfate as a carbonylation reagent, methylation Reagents and other valuable chemical products are widely used in the synthesis of high-performance resins, pharmaceuticals, and pesticide intermediates; they can replace various toxic solvents as solvents for paints and paints; Butyl ether (MTBE) also has a very broad prospect as a gasol...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J35/04C07C68/00C07C69/96
Inventor 曹勇戴维林范康年
Owner FUDAN UNIV
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