Method for controllable synthesis of methyl acetate and acetic acid by dimethyl ether carbonylation
A technology of methyl acetate and dimethyl ether, which is applied in the direction of carbon monoxide reaction to prepare carboxylic acid, carbon monoxide or formate reaction preparation, organic chemistry, etc. It can solve the problems affecting the life of the catalyst and achieve the effect of low catalyst wear
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Embodiment 1
[0025] Embodiment 1: the preparation of carbonylation catalyst
[0026] Sodium type MOR molecular sieve raw powder (SiO 2 / Al 2 o 3 =24.2) Exchanged 3 times with ammonium nitrate solution (1.0mol / L) in a water bath at 85°C, dried in an oven at 110°C after the exchange, and calcined in a muffle furnace at 550°C for 4 hours to obtain the raw powder of H-MOR molecular sieve.
[0027] The H-MOR molecular sieve powder was exchanged once with copper nitrate solution (1.0mol / L) in a water bath at 80°C, dried in an oven at 110°C after the exchange, and calcined in a muffle furnace at 550°C for 4 hours to obtain Cu-H-MOR Molecular sieve raw powder.
[0028] Take by weighing Cu-H-MOR molecular sieve former powder 38.5kg, aluminum sol 33.2kg (30.5wt.%Al 2 o 3 ) and an appropriate amount of deionized water, mixed evenly, and rolled into a 2mm spherical catalyst to obtain Cu-H-MOR-Al 2 o 3 Spherical molecular sieve catalyst, numbered CuM-03.
Embodiment 2
[0029] Embodiment 2: Carbonylation reaction activity evaluation on the catalyst
[0030] Use the numbering as CuM-03 catalyst in the embodiment 1 to carry out the carbonylation reaction on the moving bed, the reaction conditions are as follows: the catalyst loading is 1.0kg, the carbonylation reactor inventory is 0.5kg, fresh carbonylation catalyst and regeneration back catalyst from the reaction Added at the top of the reactor, as the reaction proceeds, the catalyst bed moves down very slowly, and the coke catalyst slowly flows out from the bottom of the carbonylation reactor into the regeneration reactor for charcoal regeneration, the catalyst is 0.15kg / day. The carbonylation reaction temperature and pressure are 300°C and 5MPa, and the regeneration reaction temperature and pressure are 450°C and 5MPa. Carbon monoxide / dimethyl ether / hydrogen / water in the raw material = 10 / 1 / 1 / 0.1, the total volume space velocity of the raw material gas is 5200h -1 The raw material is fed fr...
Embodiment 3
[0035] Example 3: Activity Evaluation of Carbonylation Reaction on Catalyst
[0036] Use the numbering as CuM-03 catalyst in the embodiment 1 to carry out the carbonylation reaction on the moving bed, the reaction conditions are as follows: the catalyst loading is 1.0kg, the carbonylation reactor inventory is 0.5kg, fresh carbonylation catalyst and regeneration back catalyst from the reaction Added at the top of the reactor, as the reaction proceeds, the catalyst bed moves down very slowly, and the coke catalyst slowly flows out from the bottom of the carbonylation reactor into the regeneration reactor for charcoal regeneration, the catalyst is 0.15kg / day. The carbonylation reaction temperature and pressure are 320°C and 5.5MPa, and the regeneration reaction temperature and pressure are 500°C and 5.5MPa. Carbon monoxide / dimethyl ether / hydrogen / water in the raw material = 10 / 1 / 1.5 / 0.1, the total volume space velocity of the raw material gas is 5200h -1 The raw material is fed ...
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