Method for producing oxalic ester by CO coupling
An oxalate and coupling technology, applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, metal/metal oxide/metal hydroxide catalysts, etc. Problems such as low utilization rate of nitrate and low space-time yield
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Embodiment 1
[0024] CO coupling catalyst preparation:
[0025] Dissolve ferric nitrate in water, heat to 80 °C, and impregnate in 5 mm of α-Al by vacuum rotation 2 o 3 pellets, and then dried at 120°C for 4 hours. Dissolve potassium nitrate and palladium nitrate in water respectively, adjust the solution with HCl to make the pH value about 4, then heat the solution to 80°C, and continue to immerse in 5 mm of α-Al 2 o 3 Then dry at 140°C for 4 hours, then bake at 450°C for 4 hours, and drop to room temperature to obtain the desired catalyst, whose weight composition is: 0.45%Pd+0.40%K+0.22%Fe / α-Al 2 o 3 .
[0026] CO and methyl nitrite first enter the coupling reactor to contact with the palladium-containing catalyst, and react to generate reaction effluent I containing nitrogen oxides and dimethyl oxalate; after the reaction effluent I is separated, dimethyl oxalate is obtained. Reaction effluent II and gas phase reaction effluent III containing nitrogen oxides; gas phase reaction ef...
Embodiment 2
[0029] According to the various steps and conditions of Example 1, the weight composition is as follows: 0.30%Pd+0.2%Bi+0.02%Fe / α-Al 2 o 3 palladium-containing catalyst.
[0030] CO and methyl nitrite first enter the coupling reactor to contact with the palladium-containing catalyst, and react to generate reaction effluent I containing nitrogen oxides and dimethyl oxalate; after the reaction effluent I is separated, dimethyl oxalate is obtained. Reaction effluent II and gas phase reaction effluent III containing nitrogen oxides; gas phase reaction effluent III containing nitrogen oxides and O 2 And methanol, after entering the regeneration reactor to react, generate the effluent IV containing methyl nitrite and methanol; the effluent IV containing methyl nitrite and methanol enters the water washing tower to contact with water, and the methyl nitrite is desorbed from the methanol solution , to obtain gas-phase effluent V and liquid-phase effluent VI containing methyl nitrite...
Embodiment 3
[0033] According to the various steps and conditions of Example 1, the weight composition is as follows: 0.6%Pd+0.2%Cu+0.08%Fe / α-Al 2 o 3 palladium-containing catalyst.
[0034] CO and methyl nitrite first enter the coupling reactor to contact with the palladium-containing catalyst, and react to generate reaction effluent I containing nitrogen oxides and dimethyl oxalate; after the reaction effluent I is separated, dimethyl oxalate is obtained. Reaction effluent II and gas phase reaction effluent III containing nitrogen oxides; gas phase reaction effluent III containing nitrogen oxides and O 2 And methanol, after entering the regeneration reactor to react, generate the effluent IV containing methyl nitrite and methanol; the effluent IV containing methyl nitrite and methanol enters the water washing tower to contact with water, and the methyl nitrite is desorbed from the methanol solution , to obtain gas-phase effluent V and liquid-phase effluent VI containing methyl nitrite;...
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