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 dimethyl ether carbonylation to prepare methyl acetate, can solve the problems of non-continuous production of methyl acetate, fast deactivation of mordenite molecular sieve, poor stability, etc., and achieve continuity and stability, high methyl acetate selectivity, and high initial activity

Active Publication Date: 2020-09-22
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI +2
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Problems solved by technology

At present, the dimethyl ether carbonylation method to prepare methyl acetate mainly adopts mordenite molecular sieve. Although the cost of producing methyl acetate is reduced, the mordenite molecular sieve deactivates quickly and the stability is still relatively poor. In the process of preparing methyl acetate Still need to replace the catalyst frequently, cannot produce methyl acetate continuously for a long time

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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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preparation example Construction

[0028] The present invention has no special limitation on the source of the hydrogen-type clinoptilolite. In the embodiment of the present invention, the preparation method of the hydrogen-type clinoptilolite preferably includes the following steps:

[0029] (1) Sodium-potassium clinoptilolite is immersed in an ammonium nitrate aqueous solution, and ion exchange is performed to obtain ammonium clinoptilolite;

[0030] (2) The ammonium-type clinoptilolite is sequentially dried and roasted to obtain the hydrogen-type clinoptilolite.

[0031] In the present invention, the sodium-potassium clinoptilolite is preferably immersed in an ammonium nitrate aqueous solution for ion exchange to obtain the ammonium clinoptilolite. In the present invention, in the ion exchange process, the balance cation (Na + 、K + ) and NH 4 + exchanged to obtain ammonium clinoptilolite.

[0032] In the present invention, the particle size of the sodium-potassium clinoptilolite is preferably 1-10 μm, m...

Embodiment 1

[0055] (1) Take 50g of sodium-potassium clinoptilolite (Luoyang Jianlong Micro-Na New Material Co., Ltd., model H-06) and add it to 1500mL of NH with a concentration of 1mol / L 4 NO 3 In an aqueous solution, ion-exchange at a constant temperature of 80° C. for 5 hours, and then the obtained product is washed with deionized water and dried, and the above-mentioned ion-exchange process is repeated twice to obtain ammonium-type clinoptilolite; the ammonium-type clinoptilolite is ℃ drying for 12 hours, and then roasting at 540 ℃ for 6 hours in an air atmosphere to obtain hydrogen-type clinoptilolite; the hydrogen-type clinoptilolite has an 8-membered pore structure and an average particle size of 3 μm;

[0056] (2) Use the hydrogen-type clinoptilolite obtained in step (1) as a catalyst, put it into a fixed-bed reactor, and roast it at 500° C. for 2 h under a nitrogen atmosphere to obtain activated hydrogen-type clinoptilolite; lower the bed temperature To 190°C, control the pressu...

Embodiment 2

[0059] (1) adopt the method described in embodiment 1 to prepare hydrogen clinoptilolite;

[0060] (2) Use the hydrogen-type clinoptilolite obtained in step (1) as a catalyst, put it into a fixed-bed reactor, and roast it at 500° C. for 2 h under a nitrogen atmosphere to obtain activated hydrogen-type clinoptilolite; lower the bed temperature To 190°C, control the pressure to 1MPa, introduce a mixed gas with a molar ratio of dimethyl ether and carbon monoxide of 1:10, maintain the pressure at 1MPa, control the space velocity of the mixed gas to 1000mL / (g h), and carry out dimethyl ether carbonyl reaction to produce methyl acetate.

[0061] The reaction process of the preparation method of the present embodiment is detected, and the obtained results are shown in image 3 , in the preparation method provided in this example, the initial maximum conversion rate of dimethyl ether is 13.21%, and the initial maximum selectivity of methyl acetate is 97.43%, and the conversion rate o...

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Abstract

The invention provides a method for preparing methyl acetate by carbonylation of dimethyl ether. The method comprises the following steps: subjecting a mixed gas of dimethyl ether and carbon monoxideto carry out a dimethyl ether carbonylation reaction through activated hydrogen-type clinoptilolite to obtain methyl acetate, wherein the hydrogen-type clinoptilolite has an HEU topological structure.The method provided by the invention adopts the hydrogen-type clinoptilolite having the HEU topological structure as a catalyst, the catalyst has an 8-element pore structure, and silicon-aluminum isrelatively low, and can maintain relatively high activity for a long time in the dimethyl ether carbonylation reaction process, thereby realizing the continuity and stability of methyl acetate prepared by carbonylation of dimethyl ether, and also ensuring that methyl acetate has relatively high initial activity.

Description

technical field [0001] The invention relates to the technical field of preparing methyl acetate by carbonylation of dimethyl ether, in particular to a method for preparing methyl acetate by carbonylation of dimethyl ether. Background technique [0002] Methyl acetate, also known as methyl acetate, is one of the most widely used fatty acid esters. It has excellent performance in dissolving organic matter and is widely used in the fields of coatings, adhesives, medicine, ink and pesticide synthesis intermediates. Under normal temperature and pressure, methyl acetate is extremely volatile. As a fast-drying solvent, it can dissolve acrylic acid, vinyl, nitrocellulose, polyurethane, phenolic resin, epoxy polyester and other organic compounds and resins. The demand for methyl acetate at home and abroad continues to increase. [0003] In the traditional production process of methyl acetate, acetic acid and methanol are mostly used as raw materials, and concentrated sulfuric acid i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/37B01J29/70B01J37/30
CPCB01J29/70B01J37/30C07C67/37C07C69/14
Inventor 樊卫斌许静闫文付魏渝伟李俊汾王建国董梅于吉红徐如人
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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