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Dimethyl ether carbonylation catalyst, and preparation method and application thereof
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A technology of carbonylation catalyst and dimethyl ether, which is applied in the field of catalytic chemistry and can solve the problems of catalyst carbon deposition and deactivation
Active Publication Date: 2013-06-26
YANCHANG ZHONGKE (DALIAN) ENERGY TECH CO LTD
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Avelino Corma (J.AM.CHEM.SOC.2008, 130, 16316) showed through theoretical calculations that the dimethyl ether carbonylation reaction is mainly carried out in the 8-membered ring channel, while the 12-membered ring channel is more likely to undergo side reactions, resulting in catalyst Carbon Deactivation
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Embodiment 1
[0022] Embodiment 1: the preparation of catalyst
[0023] Weigh the copper salt of orientation Amol, add deionized 100ml, then add B mol complexing agent, stir evenly to form a copper complex solution, add Cg of hydrogen-type mordenite, stir evenly, the obtained solid sample is washed, After centrifugal separation, drying and roasting, the catalyst for the carbonylation of dimethyl ether to produce methyl acetate is obtained. The catalyst numbers and preparation conditions are shown in Table 1 below, wherein #1 is unmodified hydrogen mordenite.
[0024] Table 1
[0025]
[0026] *: Determined by XRF.
[0027] Note: the ammoniacal liquor adopts the ammoniacal liquor whose concentration of ammonia by weight is 25%, and its molar quantity in the table is calculated by the ammoniacal liquor in the ammoniacal liquor.
Embodiment 2
[0028] Embodiment 2: the reactivity performance of catalyst
[0029] The 40-60-mesh sample obtained by tableting, crushing and sieving the catalyst powder obtained in Example 1 was used to measure the reaction performance of dimethyl ether carbonylation to produce methyl acetate. 0.6g of catalyst was loaded into the reactor, and a mixture of dimethyl ether, hydrogen, carbon monoxide and argon was passed through the reactor at a temperature of 220° C., a pressure of 30 atm, and a space velocity of 1500 ml / g / h. Among them, the gas flow rate F(H 2 +DME)=6.5ml / min, DME / H 2 =8.08 / 91.92 (volume ratio); gas flow F(CO+Ar)=8.5ml / min, CO / Ar=96 / 4 (volume ratio). The reaction results of each catalyst are listed in Table 2.
[0030] Table 2
[0031]
[0032] a: The highest conversion rate during the reaction.
[0033] b: Selectivity to methyl acetate when the highest conversion is reached during the reaction.
[0034] c: The time elapsed from the highest conversion rate to half of...
Embodiment 3
[0036] Reaction performance under different reaction temperatures on the 7# catalyst, other reaction conditions are the same with embodiment 2, only change reaction temperature. The reaction results are listed in Table 3.
[0037] table 3
[0038]
[0039] a: The highest conversion rate during the reaction.
[0040] b: Selectivity to methyl acetate when the highest conversion is reached during the reaction.
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Abstract
The invention provides a dimethyl ethercarbonylation catalyst, and a preparation method and application thereof. The dimethyl ethercarbonylation catalyst is a copper-complex-modified hydrogen-type mordenitemolecular sieve catalyst. The preparation method of the catalyst is implemented by using a copper complex as an ion exchange substance to modify the hydrogen-type mordenite. The preparation method comprises the following steps: (1) adding a certain amount of complexing agent into a coppersalt water solution to form a copper complex solution; (2) adding a certain amount of hydrogen-type mordenite into the copper complex solution obtained in the step (1), and uniformly stirring; and (3) washing the solid sample obtained in the step (2), carrying out centrifugal separation, drying and roasting to obtain the dimethyl ethercarbonylation catalyst for producing methyl acetate. The complexing agent selectively exchanges ions with B acid in the 12-element ring pores of the mordenite, thereby enhancing the conversion rate and selectivity of the methyl acetate preparation reaction and greatly prolonging the lifetime of the catalyst.
Description
technical field [0001] The invention belongs to the technical field of catalytic chemistry, and relates to the modification of mordenite and its application in dimethyl ether carbonyl reaction. Background technique [0002] Methyl acetate is an important organic chemical raw material. It is a raw material for preparing acetic acid, acetic anhydride, methyl acrylate, vinyl acetate and acetamide. At present, the preparation of methyl acetate comes from the esterification reaction of acetic acid and methanol. The production of acetic acid requires the use of noble metals Ir or Rh, and the HI generated during the reaction can corrode the device. Solidacid catalyzed carbonylation of dimethyl ether to produce methyl acetate is a novel route. The raw material for the reaction is DME, and currently there is an excess capacity of DME. Therefore, the carbonylation reaction of DME can improve the utilization value of DME and realize the optimal utilization of DME. [0003] At present...
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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/24B01J37/02C07C67/37C07C69/12
Inventor 刘世平朱文良刘红超刘勇刘中民孟霜鹤李利娜周慧
Owner YANCHANG ZHONGKE (DALIAN) ENERGY TECH CO LTD
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