Method for producing oxalate by coupling carbon monoxide(CO)
An oxalate ester and coupling technology, which is applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problems of low selectivity of oxalate ester and low utilization rate of nitrite ester, so as to avoid thermal or catalytic decomposition , the effect of good technical effect
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[0019] [Example 1]
[0020] Using CO and methyl nitrite as raw materials, the molar ratio of CO to methyl nitrite is 1.2:1, using palladium-supported alumina as a catalyst, and the weight content of metal palladium is 1.5% based on the weight of the carrier. The raw materials of CO and methyl nitrite first enter the crystallizer, and the water and alcohol are removed at a temperature of -20°C. The obtained effluent I enters the coupling reactor at a reaction temperature of 120°C and a reaction pressure of -0.05MPa. Airspeed is 1000 hours -1 It is contacted with a palladium-containing catalyst under the conditions of 2 to generate a reaction effluent containing dimethyl oxalate. The reaction result is: a single-pass conversion rate of CO is 62.3%, and the selectivity of dimethyl oxalate is 98.2%.
Example Embodiment
[0021] [Example 2]
[0022] Using CO and methyl nitrite as raw materials, the molar ratio of CO to methyl nitrite is 1.5:1, using palladium-supported alumina as a catalyst, and the weight content of metal palladium is 0.5% based on the weight of the carrier. The raw materials of CO and methyl nitrite enter the crystallizer first, and the water and alcohol are removed at a temperature of -10°C. The obtained effluent I enters the coupling reactor at a reaction temperature of 130°C, a reaction pressure of 0.05 MPa, and a reaction empty. 2000 hours -1 It is contacted with a palladium-containing catalyst under the conditions of, and a reaction effluent containing dimethyl oxalate is generated. The reaction result is: a single-pass conversion of CO is 55.4%, and the selectivity of dimethyl oxalate is 97.9%.
Example Embodiment
[0023] [Example 3]
[0024] Using CO and ethyl nitrite as raw materials, where the molar ratio of CO to ethyl nitrite is 1:1, and the palladium-supported ZSM-5 molecular sieve is used as the catalyst (the Si / Al molar ratio is 550:1), and the weight of the carrier As a benchmark, the weight content of metal palladium is 0.8%. The raw materials of CO and ethyl nitrite enter the cooler first, and the water and alcohol are removed at a temperature of -8°C. The obtained effluent I enters the coupling reactor where it reacts. The temperature is 140℃, the reaction pressure is 0.1MPa, and the reaction space velocity is 3000 hours -1 The reaction effluent containing diethyl oxalate is produced by contacting with the palladium-containing catalyst under the conditions of, and the reaction result is: the single-pass conversion rate of CO is 66.4%, and the selectivity of diethyl oxalate is 99.1%.
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