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A preparing method of a ZSM-35 molecular sieve catalyst used for dimethyl ether carbonylation

A technology of ZSM-35 and molecular sieve, which is applied in the field of preparation of ZSM-35 molecular sieve catalyst for dimethyl ether carbonylation, can solve the problems of only 11%, not involving the application of ZSM-35 molecular sieve, and not applying ZSM-35 molecular sieve, etc. To achieve the effect of improving catalytic activity

Inactive Publication Date: 2014-11-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under the reaction conditions of 200°C, 1Mpa, DME / CO / N2 / He=5 / 50 / 2.5 / 42.5, 12.5ml / min, the selectivity of methyl acetate reaches 96%, but the conversion rate of dimethyl ether is only Therefore, this type of molecular sieve needs to be modified urgently to improve its catalytic activity under the premise of maintaining good stability.
[0006] In the above publications, only the ZSM-35 molecular sieve with FER structure is applied to the carbonylation reaction of dimethyl ether, and the application of the modified ZSM-35 molecular sieve is not involved, and some new modification methods are not applied to ZSM -35 molecular sieve

Method used

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  • A preparing method of a ZSM-35 molecular sieve catalyst used for dimethyl ether carbonylation
  • A preparing method of a ZSM-35 molecular sieve catalyst used for dimethyl ether carbonylation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 20g of H-type ZSM-35 molecular sieve in 120ml of sodium hydroxide with a concentration of 0.4mol / L and a mixed solution of cetyltrimethylammonium bromide (CTAB) with a concentration of 0.04mol / L, at 80°C Heated in a water bath for 4 hours, filtered and washed until neutral, dried at 110°C, and calcined at 540°C for 6 hours. The prepared molecular sieve was exchanged with 1 mol / L ammonium nitrate solution three times (1 hour / time), washed with water twice (1 hour / time), and calcined to prepare catalyst Cat-D. Gained catalyst detects through XRF, and the Na in this catalyst 2 O is less than 0.05 wt%.

Embodiment 2

[0028] Put 20g H-type ZSM-35 molecular sieve in 120ml concentration of 0.3mol / L potassium hydroxide and concentration of 0.08mol / L tetradecyltrimethylammonium bromide (TTAB) mixed solution, at 80°C Heated in a water bath for 4 hours, filtered and washed until neutral, dried at 110°C, and calcined at 540°C for 6 hours. The prepared molecular sieve was exchanged with 1 mol / L ammonium nitrate solution three times (1 hour / time), washed with water twice (1 hour / time), and the catalyst Cat-E was obtained after roasting. Gained catalyst detects through XRF, and the Na in this catalyst 2 O is less than 0.05 wt%.

Embodiment 3

[0030]Put 20g of H-type ZSM-35 molecular sieve in 120ml of sodium hydroxide with a concentration of 0.8mol / L and a mixed solution of dodecyltrimethylammonium bromide (DTAB) with a concentration of 0.08mol / L, at 80°C Heated in a water bath for 4 hours, filtered and washed until neutral, dried at 110°C, and calcined at 540°C for 6 hours. The prepared molecular sieve was exchanged with 1 mol / L ammonium nitrate solution three times (1 hour / time), washed with water twice (1 hour / time), and calcined to obtain catalyst Cat-F. Gained catalyst detects through XRF, and the Na in this catalyst 2 O is less than 0.05 wt%.

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Abstract

A preparing method of a ZSM-35 molecular sieve catalyst used for dimethyl ether carbonylation is provided. The method includes step of: treating a Na-type ZSM-35 molecular sieve with an ammonium nitrate solution, washing with water, drying and calcinating to obtain an H-type molecular sieve; heating the H-type ZSM-35 molecular sieve in an alkali having a concentration of 0.1-1.0 mol / L and a mixed solution of organic surfactants with different chain lengths with a water bath at 40-90 DEG C for 0.5-6 h; washing the obtained product until the product is neutral; and exchanging with an ammonium nitrate solution, filtering, washing with deionized water, drying and calcinating to obtain an H-type catalyst. When compared with unmodified ZSM-35 molecular sieve catalysts or ZSM-35 molecular sieve catalysts modified only with the alkali, the ZSM-35 molecular sieve catalyst modified with the alkali and the mixed solution of the organic surfactants with the different chain lengths is obviously improved in catalytic activity under the premise of maintaining stability.

Description

technical field [0001] The invention belongs to the field of molecular sieve catalysts, and in particular relates to a preparation method of a ZSM-35 molecular sieve catalyst for dimethyl ether carbonylation. Background technique [0002] Methyl acetate is a fine chemical product with a wide range of uses. It has excellent solubility and a wide range of uses. It is a very important organic chemical raw material and an excellent industrial solvent. It has gradually become a mature product in the world. In place of acetone, butanone, ethyl acetate, cyclopentane, etc. The downstream products of methyl acetate mainly include acetic acid, acetic anhydride, methyl acrylate, vinyl acetate and acetamide. With the deepening of research, the production process of methyl acetate has been greatly developed. As far as the traditional process is concerned, the method of reacting methanol and acetic acid under the catalysis of concentrated sulfuric acid to generate methyl acetate is most...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40C07C69/14C07C67/37
Inventor 刘盛林刘小行李秀杰徐龙伢谢素娟张大洲
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI