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Composite oxide load type catalyst and preparation process thereof

A supported catalyst, composite oxide technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, preparation of organic compounds, etc., can solve problems such as unreported

Inactive Publication Date: 2009-06-10
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, this method has not been used in the world to prepare CuCl / TiO 2 -SiO 2 , CuCl 2 / TiO 2 -SiO 2 and CuCl 2 -PdCl 2 / TiO 2 -SiO 2 Composite oxide-supported catalysts, and the research papers and patent literature on the synthesis of DMC by methanol oxidative carbonylation on these two types of catalysts have not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0021] a) Add 25 mL of tetraethyl orthosilicate to 50 mL of absolute ethanol at a temperature of 20°C, add 6 mL of deionized water and 12.5 mL of acetic acid in sequence, and stir for 1 hour for hydrolysis;

[0022] b) Add 3.3mL of titanium isopropoxide to 6.6mL of absolute ethanol at 20°C, then 1.7mL of acetic acid, stir and hydrolyze for 30 minutes, mix with pre-hydrolyzed silica sol and stir vigorously at 20°C 1 hour to make it form a transparent sol;

[0023] c) 2.2 g of purified CuCl was dissolved in 60 mL of ethanol solution, then added into the titanium silica sol, and stirred at room temperature to form a composite gel;

[0024] d) aging the gel at 20°C for 50-200 hours to form a xerogel;

[0025] e) The obtained xerogel was sintered in a muffle furnace at 550°C for 3 to 10 hours, and cooled naturally to room temperature to obtain about 9.7g of CuCl / TiO 2 -SiO 2 Composite metal oxide supported catalyst.

Embodiment approach 2

[0027] a) Add 6 mL of tetraethyl orthosilicate to 12 mL of absolute ethanol at a temperature of 20°C, add 1.5 mL of deionized water and 3 mL of acetic acid in sequence, and stir for 1 hour for hydrolysis;

[0028]b) Add 24mL of titanium isopropoxide to 48mL of absolute ethanol at 20°C, then 12mL of acetic acid, stir and hydrolyze for 30 minutes, mix with pre-hydrolyzed silica sol and stir vigorously at 20°C for 1 hour to dissolve to form a transparent sol;

[0029] c) 4.6g of purified CuCl 2 2H 2 O was dissolved in 100mL ethanol solution, then added into the titanium silica sol, and stirred at room temperature to form a composite gel;

[0030] d) aging the gel at 20°C for 50-200 hours to form a xerogel;

[0031] e) The obtained xerogel was sintered in a muffle furnace at 550°C for 3 to 10 hours, and cooled naturally to room temperature to obtain about 11.6g of CuCl 2 / TiO 2 -SiO 2 Composite metal oxide supported catalyst.

Embodiment approach 3

[0033] a) Add 20 mL of tetraethyl orthosilicate to 40 mL of absolute ethanol at a temperature of 20°C, add 5 mL of deionized water and 10 mL of acetic acid in sequence, and stir for 1 hour for hydrolysis;

[0034] b) Add 8.9mL of titanium isopropoxide to 18mL of absolute ethanol at 20°C, then 4.5mL of acetic acid, stir and hydrolyze for 30 minutes, mix with the pre-hydrolyzed silica sol and stir vigorously at 20°C for 1 hour to form a transparent sol;

[0035] c) 2.3g CuCl 2 2H 2 O and 2.3 g PdCl 2 Dissolve in 100mL ethanol solution, then add to titanium silica sol, stir at room temperature to form a composite gel;

[0036] d) aging the gel at 20°C for 50-200 hours to form a xerogel;

[0037] e) The obtained xerogel was sintered in a muffle furnace at 550° C. for 3 to 10 hours, and cooled naturally to room temperature to obtain about 11.9 g of

[0038] CuCl 2 -PdCl 2 / TiO 2 -SiO 2 Composite metal oxide supported catalyst.

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PUM

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Abstract

A composite oxide carried catalyst used for preparing dimethyl carbonate (DMC) from methanol by oxidation and oxidation is prepared through co-gelatinizing ethyl n-silicate and iso-propanol titanium while adding co-porous chloride, copper chloride and palladium chloride, ageing, drying and calcination. Its advantages are high catalytic activity and selectivity and high output rate of DMC.

Description

1. Technical field [0001] The invention relates to a composite oxide supported catalyst and a preparation method thereof, which relate to a composite oxide supported catalyst for synthesizing dimethyl carbonate by oxidative carbonylation of methanol and a preparation method thereof, and belong to the technical field of organic chemical synthesis in chemical engineering. 2. Background technology [0002] Dimethyl Carbonate (Dimethyl Carbonate, referred to as DMC) is considered to be one of the most important green chemical products in the 21st century. As an intermediate, it can replace phosgene, dimethyl sulfate, methyl chloride and methyl chloroformate, etc. Toxic or carcinogenic chemicals for carbonylation, methylation, methyl esterification and transesterification and other organic synthesis reactions; in addition, due to its excellent solubility and high oxygen content, it can also be used as a high-quality solvent and fuel additive. Due to the serious harm to the enviro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J32/00B01J37/03C07C68/00
Inventor 谢克昌任军李忠鲍卫仁
Owner TAIYUAN UNIV OF TECH