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Catalyst for synthesis of diethyl oxalate employing carbon monoxide gas-phase catalytic coupling and preparation method thereof

A technology of diethyl oxalate and carbon monoxide, which is applied in the direction of carbon monoxide or formate reaction preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., can solve the problem of low space-time yield of oxalate , poor catalytic performance and other problems, to achieve the effect of high space-time yield and high reactivity

Inactive Publication Date: 2009-12-30
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the catalysts reported so far use metal palladium (Pd) as the active component, and α-Al 2 o 3 as the carrier, while SiO 2 and activated carbon as supports show poor catalytic performance (USP 4229591, 1980)
Then it was reported that Pd / α-Al 2 o 3 Add Mo, Ni, Ti, Fe, Ga, Ce, Na to the catalyst 2 O and other additives are used in the process of carbon monoxide catalytic coupling to synthesize dimethyl oxalate, diethyl oxalate and diisopropyl oxalate, but the space-time yield of oxalate is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The present embodiment is the carbon monoxide gas-phase catalytic coupling synthesis diethyl oxalate catalyst (catalyst A) prepared by the impregnation method comprising the following steps:

[0025] (1) Carrier drying: carrier α-Al 2 o 3 Before use, put it in a tube furnace and dry it in a flowing nitrogen atmosphere at 300°C for 5 hours to remove the moisture on the surface. The nitrogen flow rate is 40mL min -1 ;

[0026] (2) Preparation of copper salt solution: Copper nitrate (Cu(NO 3 ) 2 ·3H 2 O) be dissolved in deionized water, stir and dissolve, and be made into the copper salt solution that contains copper ion concentration and be 0.010M;

[0027] (3) Preparation of mixed salt solution: take 100 mL of the copper salt solution obtained in the above step (2), add palladium chloride (PdCl 2 ), fully stirred to dissolve the palladium salt, to obtain a mixed salt solution, and the concentration of palladium ions in the solution was 0.020M;

[0028] (4) Prepara...

Embodiment 2

[0032] This embodiment is the carbon monoxide gas-phase catalytic coupling synthesis diethyl oxalate catalyst (catalyst B) prepared by the impregnation method comprising the following steps:

[0033] (1) Carrier drying: carrier α-Al 2 o 3 Before use, put it in a tube furnace and dry it in a flowing nitrogen atmosphere at 300°C for 5 hours to remove the moisture on the surface. The nitrogen flow rate is 40mL min -1 ;

[0034] (2) Preparation of copper salt solution: Copper nitrate (Cu(NO 3 ) 2 ·3H 2 O) be dissolved in deionized water, stir and dissolve, and be made into the copper salt solution that contains copper ion concentration and be 0.010M;

[0035](3) Preparation of mixed salt solution: take 100 mL of the copper salt solution obtained in the above step (2), add palladium chloride (PdCl 2 ), fully stirred to dissolve the palladium salt, to obtain a mixed salt solution, and the concentration of palladium ions in the solution was 0.020M;

[0036] (4) Preparation of ...

Embodiment 3

[0040] The present embodiment is the carbon monoxide gas-phase catalytic coupling synthesis diethyl oxalate catalyst (catalyst C) prepared by the impregnation method comprising the following steps:

[0041] (1) Carrier drying: carrier α-Al 2 o 3 Before use, put it in a tube furnace and dry it in a flowing nitrogen atmosphere at 300°C for 5 hours to remove the moisture on the surface. The nitrogen flow rate is 40mL min -1 ;

[0042] (2) Preparation of copper salt solution: Copper nitrate (Cu(NO 3 ) 2 ·3H 2 O) be dissolved in deionized water, stir and dissolve, and be made into the copper salt solution that contains copper ion concentration and be 0.010M;

[0043] (3) Preparation of mixed salt solution: take 100 mL of the copper salt solution obtained in the above step (2), add palladium chloride (PdCl 2 ), fully stirred to dissolve the palladium salt, to obtain a mixed salt solution, and the concentration of palladium ions in the solution was 0.020M;

[0044] (4) Prepara...

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PUM

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Abstract

The invention discloses a catalyst for the synthesis of diethyl oxalate employing carbon monoxide gas-phase catalytic coupling and the catalyst adopts metal palladium as active component, alpha-Al2O3 as carrier and transition metal copper as promoter; wherein, the content of metal palladium is 0.1-5.0% of the carrier and the content of transition metal copper is 0.05-3.0%. The catalyst shows higher reactivity and higher time space yield of dimethyl oxalate in the reaction that carbon monoxide and ethyl nitrite are used to synthesize dimethyl oxalate. The invention also discloses a preparation method of the catalyst.

Description

technical field [0001] The invention belongs to the technical field of diethyl oxalate preparation, and in particular relates to a carbon monoxide gas-phase catalytic coupling synthesis diethyl oxalate catalyst and a preparation method thereof. Background technique [0002] Diethyl oxalate, also known as Diethyl Oxalate, has the molecular formula C 6 h 10 o 4 ; It is an important chemical raw material, which is widely used in the preparation of various dyes, medicines, important solvents, extractants and various intermediates. In the 21st century, oxalate, as a degradable and environmentally friendly engineering plastic monomer, has received extensive attention internationally. Low-pressure hydrogenation of oxalate can produce ethylene glycol, an important chemical raw material, oxalic acid can be produced by normal-pressure hydrolysis, and high-quality fertilizer oxamide can be obtained by normal-pressure ammonia solution. [0003] The traditional production of diethyl ...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C69/36C07C67/36
Inventor 李扬胡玉容王科范鑫袁小金许红云
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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