A kind of chlorine-free cuy catalyst for synthesizing dimethyl carbonate and its preparation method and application
A technology of dimethyl carbonate and catalyst, which is applied in the field of catalyst and preparation, can solve problems such as catalyst deactivation, equipment corrosion, and environmental pollution, and achieve the effects of overcoming catalyst deactivation, good catalytic performance, and avoiding the use of a large amount of solvents
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Embodiment 1
[0032] (1) take by weighing the NaY molecular sieve (SiO 2 / Al 2 o 3 =5.3, specific surface area 810m 2 / g, pore volume 1.1cm 3 g -1 ) 5g and 0.5mol / L ammonium nitrate solution 50mL, exchange at 80°C for 12h, repeat the exchange twice, wash, filter with suction, and dry at 100°C to obtain NH 4 Y molecular sieve, its exchange degree reaches 78%.
[0033] (2) Weigh 3gNH 4 Y and 1.227 g of copper acetylacetonate were uniformly mixed mechanically, and steam impregnation was carried out at 150° C. for 24 hours to obtain a catalyst precursor.
[0034] (3) Weigh 3 g of the catalyst precursor, raise the temperature to 400° C. for 18 hours in the air at a heating rate of 3° C. / min and activate for 18 hours to obtain a catalyst. The loading amount of Cu is 10 wt % in terms of metal.
[0035] See attached table 1 for the reaction conditions and reactivity evaluation results of direct vapor-phase oxidative carbonylation of methanol to dimethyl carbonate by the catalyst. The specifi...
Embodiment 2
[0038] (1) take by weighing the NaY molecular sieve (SiO 2 / Al 2 o 3 =4.8, specific surface area 760m 2 / g, pore volume 1.2cm 3 g -1 ) 5g and 0.2mol / L ammonium nitrate solution 50mL, exchanged at 30°C for 4h, repeated the exchange once, washed, suction filtered, and dried at 100°C to obtain NH 4 Y molecular sieve, its exchange degree reaches 32%. (2) Weigh 3gNH 4 Y and 0.982 g of copper acetylacetonate were uniformly mixed mechanically, sublimated and impregnated at 250° C. for 8 hours to obtain a catalyst precursor.
[0039] (3) Weigh 3g of catalyst precursor, in 50vol%N 2 +50vol%O 2 In the atmosphere, the temperature was raised to 700° C. for 8 hours at a heating rate of 3° C. / min for activation to obtain a catalyst, and the loading amount of Cu was 8 wt % in terms of metal.
[0040] Catalyst in direct vapor phase oxidative carbonylation of methanol to synthesize dimethyl carbonate The reaction conditions and activity evaluation activity are shown in attached table ...
Embodiment 3
[0042] (1) Weigh the NaY molecular sieve (SiO 2 / Al 2 o 3 =11, the specific surface area is 655m 2 / g, pore volume 0.8cm 3 g -1 ) 5g and 0.1mol / L ammonium nitrate solution 50mL, exchanged at 40°C for 8h, repeated the exchange twice, washed, suction filtered, and dried at 100°C to obtain NH 4 Y molecular sieve, its exchange degree reaches 42%.
[0043] (2) Weigh 3gNH 4 Y and 0.736 g of copper acetylacetonate were uniformly mixed mechanically, sublimated and impregnated at 250° C. for 4 hours to obtain a catalyst precursor.
[0044] (3) Weigh 3 g of the catalyst precursor, heat it up to 750° C. for 4 hours in Ar at a heating rate of 5° C. / min, and activate it for 4 hours to obtain a catalyst. In terms of metal, the Cu loading is 6 wt%.
[0045] Catalyst in direct vapor phase oxidative carbonylation of methanol to synthesize dimethyl carbonate The reaction conditions and activity evaluation activity are shown in attached table 1, and the specific steps are shown in Example...
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