Catalyst for catalyzing methanol carbonylation, preparation method of catalyst and method for preparing acetic acid and methyl acetate by methanol carbonylation
A technology of methanol carbonylation and methyl acetate, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, carbon monoxide reaction to prepare carboxylic acid, etc. , the reactivity and lifespan are not ideal, etc., to achieve the effect of high yield, high conversion rate and high stability
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Embodiment 1
[0049] A catalyst for catalyzing the carbonylation of methanol, which is prepared by the following method:
[0050] Weigh 5.72g of nickel nitrate, dissolve in 20g of distilled water, slowly add 10g of SiO2 under slow stirring 2 In this method, after ultrasonic impregnation for 1 hour, standing at room temperature for impregnation for 24 hours, drying at 80°C for 8 hours, drying at 120°C for 16 hours, and roasting at 500°C for 3 hours to obtain a catalyst precursor.
[0051] Catalyst precursor in 20vol1% CH 4 -80vo1%H 2 In the mixed gas, reduce at 350 ℃ for 4h, that is.
[0052] Methanol carbonylation was carried out in a pressurized continuous fixed-bed reactor to prepare acetic acid and methyl acetate, and the activity of the catalyst prepared in this example for catalyzing methanol carbonylation was evaluated.
[0053] The specific operation is as follows: before the reaction, the catalyst (6 mL) was first reduced in hydrogen at 300° C. for 3 h, and then the temperature o...
Embodiment 2
[0060] A catalyst for catalyzing the carbonylation of methanol, which is prepared by the following method:
[0061] Weigh 8.58g of nickel nitrate, dissolve it in 15g of distilled water, slowly add 10g of Al under slow stirring 2 o 3 In , after ultrasonic impregnation for 3 hours, it was impregnated at room temperature for 36 hours, then dried at 100°C for 24 hours, and calcined at 550°C for 5 hours to obtain a catalyst precursor.
[0062] Catalyst precursor using 10vol1% ethane-90vol1% H 2 In the mixed gas, reduce it at 390°C for 5h to get it.
[0063] The method provided in Example 1 was used to evaluate the activity of the catalyst for methanol carbonylation provided in this example.
[0064] The specific reaction conditions are as follows: at 250° C., 5 MPa, the feed rate of hydrogen is 222 mL / min, the feed rate of CO is 111 mL / min, and the feed rate of methanol is 0.2 mL / min.
[0065] When reacting for 72 hours, it was measured that the conversion rate of methanol was ...
Embodiment 3
[0067] A catalyst for catalyzing the carbonylation of methanol, which is prepared by the following method:
[0068] Weigh 4.66g of nickel chloride, dissolve it in 12g of distilled water, slowly add it into 10g of activated carbon under slow stirring, after ultrasonic impregnation for 2 hours, after impregnating at room temperature for 48 hours, first bake at 80°C for 8h, then at 120°C Baking for 24 hours for drying, and baking at 500° C. for 6 hours in a nitrogen atmosphere to obtain a catalyst precursor.
[0069] Catalyst precursor in 10vol1% butane-90vol1% H 2 The mixed gas was reduced at 400°C for 6h to obtain.
[0070] The method provided in Example 1 was used to evaluate the activity of the catalyst for methanol carbonylation provided in this example.
[0071] The specific reaction conditions are as follows: at 290° C., 6 MPa, the feed rate of hydrogen is 222 mL / min, the feed rate of CO is 111 mL / min, and the feed rate of methanol is 0.2 mL / min.
[0072] When reacting ...
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