Method for preparing methyl methacrylate by dehydrogenation esterification of isobutyric acid
A technology of methyl methacrylate and isobutyric acid is applied in the preparation of carboxylate, chemical instruments and methods, catalyst activation/preparation, etc., and can solve the problems of insufficient market competitiveness, low selectivity, and many by-products. , to achieve the effect of more dehydrogenation active centers, increase product yield, and reduce reaction steps
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Embodiment 1
[0023] (1) Dissolve ammonium molybdate into methanol to obtain solution A, dissolve 2-methylimidazole into methanol to obtain solution B, slowly add solution A to solution B under vigorous stirring, and continue stirring for 1 h. The molar ratio of molybdenum atom to 2-methylimidazole was 1:5.
[0024] (2) Transfer the above solution to an autoclave with a polytetrafluoroethylene lining, and react at 100° C. for 24 hours. After cooling, take out, filter, wash with methanol, and vacuum dry at 50 °C for 20 h to obtain catalyst precursor M / ZIF.
[0025] (3) The precursor M / ZIF was placed in a quartz tube, and 120ml / min of NH was introduced 3 / N 2 The mixed gas was calcined at 700 °C for 3 h to obtain a MN / N-C bifunctional catalyst. The mixed gas NH 3 / N 2 The ratio is 15:1.
[0026] (4) 0.2g of catalyst is loaded into the fixed bed reactor, and the isobutyric acid and methanol mixed solution whose mass ratio is 1:8 is added, and N 2 The reaction temperature is 400℃, the pre...
Embodiment 2
[0028] (1) Dissolve ammonium tungstate into methanol to obtain A, dissolve 2-methylimidazole into methanol to obtain solution B, slowly add solution A to solution B dropwise with vigorous stirring, and continue stirring for 1 h. The molar ratio of molybdenum atom to 2-methylimidazole is 1:8.
[0029] (2) Transfer the above solution into an autoclave with a polytetrafluoroethylene lining, and react at 80° C. for 36 hours. After cooling, take out, filter, wash with methanol, and vacuum dry at 80 °C for 16 h to obtain catalyst precursor M / ZIF.
[0030] (3) The precursor M / ZIF was placed in a quartz tube, and 120ml / min of NH was introduced 3 / N 2 The mixed gas was calcined at 800 °C for 4 h to obtain the MN / N-C bifunctional catalyst. Mixed gas NH 3 / N 2 The ratio is 12:1.
[0031] (4) 0.2g of catalyst is loaded into the fixed bed reactor, and the isobutyric acid and methanol mixed solution whose mass ratio is 1:8 is added, and N 2 The reaction temperature is 400℃, the press...
Embodiment 3
[0033] (1) Dissolve ammonium molybdate and cobalt nitrate into methanol to obtain A, dissolve 2-methylimidazole into methanol to obtain solution B, slowly add solution A to solution B dropwise with vigorous stirring, and continue stirring for 1 h. The molar ratio of the sum of molybdenum + cobalt atoms to 2-methylimidazole is 1:10, and the molybdenum atom to cobalt atom ratio is 1:1.
[0034] (2) Transfer the above solution to an autoclave with a polytetrafluoroethylene lining, and react at 120° C. for 24 hours. After cooling, take out, filter, wash with methanol, and vacuum dry at 40 °C for 20 h to obtain catalyst precursor M / ZIF.
[0035] (3) The precursor M / ZIF was placed in a quartz tube, and 100ml / min of NH was introduced 3 / N 2 The mixed gas was calcined at 600 °C for 5 h to obtain the MN / N-C bifunctional catalyst. Mixed gas NH 3 / N 2 The ratio is 10:1.
[0036] (4) 0.2 g of catalyst is loaded into the fixed bed reactor, and the isobutyric acid and methanol mixed s...
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