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A kind of method for preparing methyl acetate by carbonylation of dimethyl ether

A technology of methyl acetate and dimethyl ether, which is applied in the field of catalytic chemistry, can solve the problems of uneven temperature distribution of the catalyst bed, difficult industrial production, and difficult control, so as to avoid hot spots, improve selectivity, and prolong catalyst life. Effect

Active Publication Date: 2016-01-06
YANCHANG ZHONGKE (DALIAN) ENERGY TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of industrialization of the above reactors, the temperature distribution of the catalyst bed is uneven and difficult to control, making it difficult to carry out large-scale industrial production

Method used

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  • A kind of method for preparing methyl acetate by carbonylation of dimethyl ether
  • A kind of method for preparing methyl acetate by carbonylation of dimethyl ether
  • A kind of method for preparing methyl acetate by carbonylation of dimethyl ether

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Experimental program
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Effect test

Embodiment 1

[0029] The preparation of embodiment 1 catalyst

[0030] The catalyst is represented by n% M / S, where:

[0031] Molecular sieves: S = mordenite (MOR), ferrierite (FER)

[0032] Heteroatoms: M = iron (Fe), gallium (Ga);

[0033] Loading metal: M = iron (Fe), copper (Cu), silver (Ag), rhodium (Rh), platinum (Pt), palladium (Pd), cobalt (Co), iridium (Ir);

[0034] n=the mass percentage of the metal in the total weight of the catalyst×100; the metal in the supported catalyst is in an oxidation state, and the content is represented by elemental metal.

[0035] 1.1 Synthesis of sodium mordenite

[0036] Dissolve 19 grams of NaOH into 40 ml of deionized water, then add a certain amount of sodium aluminate or a mixture of sodium aluminate + iron nitrate or sodium aluminate + gallium oxide, and stir until completely dissolved. Add 650ml of water to the resulting solution for dilution, then add a certain amount of SiO 2powder and stirred for 30 minutes. The resulting material was...

Embodiment 2

[0060] Embodiment 2. Catalyst pretreatment and reaction

[0061] 2.1 Conventional pretreatment of catalyst

[0062] At the beginning of the investigation, the catalyst was activated at 550°C in a nitrogen atmosphere for 4 hours, then the temperature of the bed was lowered to the reaction temperature, and a certain proportion of dimethyl ether was introduced, and the mixed gas of carbon monoxide and hydrogen was pressurized and reacted. The reactor is heated by an electric furnace, and the reaction temperature is determined by a thermocouple inserted into the catalyst bed.

[0063] 2.2 Pyridine pretreatment of mordenite

[0064] When the mordenite is used as the catalyst, the catalyst can be subjected to pyridine adsorption pretreatment before the reaction. The catalyst was activated at 550°C in a nitrogen atmosphere for 4 hours, then the temperature of the bed was lowered to 300°C, and gaseous pyridine diluted with nitrogen was introduced for adsorption. After 1 hour of ads...

Embodiment 3

[0065] Embodiment 3. the analytical method of product

[0066] The raw materials and the obtained products were analyzed by Agilent7890A gas chromatography. The chromatograph is equipped with dual detectors FID and TCD, and has a ten-way valve, which allows the products to enter the packed column and capillary column respectively at the same time. The hydrogen flame detector detects hydrocarbons, alcohols and ethers in the product, and the thermal conductivity detector detects carbon monoxide and hydrogen in the raw materials and products. Data were processed with Agilent's Chemstation software.

[0067] The specific chromatographic conditions of Agilent are as follows:

[0068] Chromatography: Agilent7890A

[0069] FID column: HP-PLOT-Q19091S-001, 50mx0.2mm (inner diameter), 0.5μm film thickness

[0070] Carrier gas: helium, 2.5ml / min

[0071] Oven temperature: 35°C for 5 minutes

[0072] 35-150°C, 5°C / min

[0073] 150℃ for 10min

[0074] Inlet: Split (50:1) Temperatu...

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Abstract

Provided is a method for preparing methyl acetate by dimethyl ether carbonylation, comprising passing a feed gas including dimethyl ether, carbon monoxide and optional hydrogen through a reactor filled with a mordenite and / or ferrierite molecular sieve based catalyst and reacting at a reaction temperature of 190-320°C, a reaction pressure of 0.5-20.0 MPa and a gas space velocity of 500-5000 h-1 so as to prepare methyl acetate, wherein the molar ratio of dimethyl ether to carbon monoxide is DME / CO=1 / 1-1 / 15, the molar ratio of hydrogen to carbon monoxide is H2 / CO=0-10 / 1, and the feed gas is distributed into each catalyst bed layer in a segmental feeding manner. A feed gas including dimethyl ether and carbon monoxide is uniformly distributed into each catalyst bed layer via a gas distributor, in a segmental feeding manner, which can remarkably improve the conversion rate of dimethyl ether, effectively control or adjust the temperature distribution of a catalyst bed layer, avoid the appearance of a hot spot, and prolong the service life of a catalyst.

Description

technical field [0001] The invention belongs to the field of catalytic chemistry, and in particular relates to a method for preparing methyl acetate. The raw material dimethyl ether enters a catalyst bed through a gas distributor, and undergoes a carbonylation reaction to synthesize methyl acetate. Background technique [0002] With the rapid development of modern industry, the contradiction between energy supply and demand has become increasingly prominent. my country, as a big energy consumer and a big energy shortage country, urgently needs to find alternative energy sources. As a clean energy source, ethanol has good miscibility and can be added to gasoline as a blending component to partially replace gasoline, increase the octane number and oxygen content of gasoline, effectively promote the complete combustion of gasoline, and reduce CO and HC emissions in vehicle exhaust. As a partial substitute of vehicle fuel, ethanol can make my country's vehicle fuel present a d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/37
CPCC07C67/37
Inventor 朱文良刘红超刘勇倪友明刘中民孟霜鹤李利娜刘世平周慧
Owner YANCHANG ZHONGKE (DALIAN) ENERGY TECH CO LTD
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