Method used for preparing methyl acetate

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

Active Publication Date: 2014-07-02
YANCHANG ZHONGKE (DALIAN) ENERGY TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the process of industrialization of the above reactors, the temperature distribution of the catalyst b

Method used

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  • Method used for preparing methyl acetate
  • Method used for preparing methyl acetate
  • Method used for preparing methyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation of embodiment 1 catalyst

[0029] Catalysts are expressed in n%M / MOR, where:

[0030] Heteroatoms: M = iron (Fe), gallium (Ga);

[0031] Loading metal: M = iron (Fe), copper (Cu), silver (Ag), rhodium (Rh), platinum (Pt), palladium (Pd), cobalt (Co), iridium (Ir);

[0032] 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.

[0033] 1.1 Synthesis of sodium mordenite

[0034] 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 placed in a Teflon-lined stainless steel reaction vessel. Cryst...

Embodiment 2

[0049] Embodiment 2. Catalyst pretreatment and reaction

[0050] 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 300°C, and gaseous pyridine diluted with nitrogen was introduced for adsorption. After 1 hour of adsorption, purging of pure nitrogen was carried out for 30 minutes at the same temperature. A certain proportion of dimethyl ether, a mixture of carbon monoxide and hydrogen is introduced to increase the pressure and react. The reactor is heated by an electric furnace, and the reaction temperature is determined by a thermocouple inserted into the catalyst bed.

Embodiment 3

[0051] Embodiment 3. the analytical method of product

[0052] The starting materials and the resulting products were analyzed using an Agilent 7890A gas chromatograph. 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.

[0053] The specific chromatographic conditions of Agilent are as follows:

[0054] Chromatography: Agilent 7890A

[0055] FID column: HP-PLOT-Q 19091S-001, 50m x 0.2mm (inner diameter), 0.5μm

[0056] film thickness

[0057] Carrier gas: helium, 2.5ml / min

[0058] Oven temperature: 35°C for 5 minutes

[0059] 35-150°C, 5°C / min

[0060] 150℃ for...

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Abstract

Provided in the present invention is a process for preparing methyl acetate through carbonylation of dimethyl ether, comprising: passing a feed gas containing dimethyl ether, carbon monoxide, and optional hydrogen gas through a reactor loaded with a mordenite molecular sieve catalyst, and preparing methyl acetate by reacting same at a reaction temperature of 19 to 320°C, a reaction pressure of 0.5 to 20.0 Mpa, and a gas volume space velocity of 500 to 5000 h-1; wherein the mordenite molecular sieve catalyst is a hydrogen-type mordenite molecular sieve catalyst with an adsorbed organic amine, the molar ratio of the dimethyl ether to carbon monoxide in the feed gas is DME/CO = 1/1 to 1/15, the molar ratio of the hydrogen gas to carbon monoxide is H2/CO = 0 to 10/1, and the dimethyl ether in the feed gas is charged into the reactor by means of feeding in stages. The present invention is characterized in that: through treatment by organic amine adsorption, the temperature distribution of catalyst bed can be effectively controlled so as to avoid the occurrence of hot points, and thereby side reactions are reduced, the selectivity of target product is improved, and the lifetime of the catalyst is greatly extended.

Description

technical field [0001] The invention relates to a method for synthesizing methyl acetate through carbonylation of dimethyl ether under mild conditions, and particularly provides a fixed-bed reactor in which molecular sieves are used as catalysts and treated with organic amines, and the raw material dimethyl ether is fed in stages. technology and its application. 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 ve...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/37
CPCC07C67/37B01J29/18C07C69/14B01J37/0203B01J2229/34
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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