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Preparation method of catalyst for synthesizing methyl ethyl ketone from isobutyraldehyde

A catalyst and methyl ethyl ketone technology, which is applied in the field of catalyst preparation, can solve the problems of unstable target product and reduced yield, and achieve the effects of good surface distribution, good structure and guaranteed catalytic activity.

Active Publication Date: 2020-12-15
RUNTAI CHEM TAIXING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN106517233A uses a fluorine-free and solvent-free route to synthesize Beta zeolite molecular sieve enriched in B form. The entire production process does not use solvents and highly toxic fluorine species, which reduces unnecessary losses in the production process, but there is no The impurities are removed, the yield is reduced, and the target product is unstable

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  • Preparation method of catalyst for synthesizing methyl ethyl ketone from isobutyraldehyde

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Preparation of catalyst

[0023] (1) Take 3.35g tetrapropylammonium bromide (TPABr), 0.014g boehmite, 1.35gNaSiO 3 9H 2 O, 1.3g ammonium chloride, 0.3gH 2 GeO 3 Put in a mortar and grind to a fine powder.

[0024] (2) Mix the raw material of step (1) with 12.63g LUDOX HS-40 (30wt% SiO 2 ) were mixed and ground for 10 minutes to obtain a precursor, which was transferred to a Teflon-lined stainless steel autoclave and kept at a temperature of 190°C for 48 hours.

[0025] (3) Cool the product of step (2) in the autoclave, filter and separate the product, wash, and calcinate the product under a constant flow of ammonia at a temperature of 600° C. for 2 hours.

[0026] (4) Cool the sample obtained in step (3) to room temperature, add 2molNaNO 3 The solution was exchanged more than three times, filtered, washed with deionized water, dried at 100°C, placed in a muffle furnace at a temperature of 550°C, and calcined for 4 hours to obtain a Ge-ZSM-5 catalyst.

[0027]...

Embodiment 2

[0030] 1) Take 3.2g tetrapropylammonium bromide (TPABr), 0.012g boehmite, 1.0gNaSiO 3 9H 2 O, 1.2g ammonium chloride, 0.1gH 2 GeO 3 Put in a mortar and grind to a fine powder.

[0031] (2) Mix the raw material of step (1) with 11.02g LUDOX HS-40 (30wt% SiO 2 ) were mixed and ground for 5 minutes to obtain a precursor, which was transferred to a Teflon-lined stainless steel autoclave and kept at a temperature of 170°C for 24 hours.

[0032] (3) Cool the product autoclave of step (2), filter and separate the product, wash, and calcinate the product under a constant ammonia flow, keep the temperature at 500°C, and keep it for 1h.

[0033] (4) Cool the sample obtained in step (3) to room temperature, add 1molNaNO 3 The solution was exchanged more than three times, filtered, washed with deionized water, dried at 120°C, placed in a muffle furnace at a temperature of 500°C, and calcined for 8 hours to obtain a Ge-ZSM-5 catalyst.

[0034] 2. Synthesis of methyl ethyl ketone (ME...

Embodiment 3

[0037](1) Take 4.21g tetrapropylammonium bromide (TPABr), 0.015g boehmite, 2.0gNaSiO 3 9H 2 O, 1.4g ammonium chloride, 0.24gH 2 GeO 3 Put in a mortar and grind to a fine powder.

[0038] (2) Mix the raw material of step (1) with 15.73g LUDOX HS-40 (30wt% SiO 2 ) were mixed and ground for 10 minutes to obtain a precursor, which was transferred to a Teflon-lined stainless steel autoclave and kept at a temperature of 200°C for 48 hours.

[0039] (3) Cool the product autoclave of step (2), filter and separate the product, wash, and calcinate the product under a constant ammonia flow, keep the temperature at 650°C for 2h.

[0040] (4) Cool the sample obtained in step (3) to room temperature, add 3molNaNO 3 The solution was exchanged more than three times, filtered, washed with deionized water, dried at 100°C, placed in a muffle furnace at a temperature of 600°C, and calcined for 8 hours to obtain a Ge-ZSM-5 catalyst.

[0041] 2. Synthesis of methyl ethyl ketone (MEK) by isom...

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Abstract

The invention belongs to the technical field of catalysts, and particularly discloses a preparation method of a catalyst for synthesizing methyl ethyl ketone (MEK) from isobutyraldehyde. The method comprises the steps of grinding raw materials to uniformly distribute the raw materials, and preparing a Ge-ZSM-5 catalyst by a one-pot solvent-free co-regulation method. Tn the preparation process, nosolvent is used, and neither pretreatment nor post-treatment is performed, thereby reducing the discharge of wastewater, and greatly simplifying the synthesis steps of the catalyst. The prepared catalyst has the advantages of good structure, uniform metal distribution, good surface distribution state, high acid strength and the like, is used for isobutyraldehyde isomerization synthesis of methyl ethyl ketone, can significantly improve the catalytic activity of the catalyst and increase the yield of methyl ethyl ketone, has an isobutyraldehyde conversion rate of 94% or above and a yield of 93%or above, and has a great application prospect.

Description

technical field [0001] The invention belongs to the technical field of catalysts, in particular to a preparation method of a catalyst used to catalyze the synthesis of methyl ethyl ketone (MEK) from isobutyraldehyde. Background technique [0002] Methyl ethyl ketone (CH 3 COCH 2 CH 3 ), also known as butanone, is a colorless and transparent liquid and is one of the downstream products of isobutyraldehyde. It is widely used in the production of organic matter such as nitrocellulose and phenolic resin. Nowadays, the production process of methyl ethyl ketone includes n-butene two-step method, n-butane liquid phase oxidation method, isobutylbenzene method and isobutyraldehyde isomerization method, etc. The isobutyraldehyde isomerization method has important applications in chemical reactions . Xu Zhanglin from Dalian Institute of Chemical Physics, Chinese Academy of Sciences reported that NH 4 F modified ZSM-5, BZSM-5 has lower acidity, which makes it less deactivated duri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/67C07C49/10B01J29/40B01J37/30
CPCC07C45/67B01J29/405B01J37/0009B01J37/0036B01J37/30B01J2229/18C07C49/10
Inventor 张世元卢小松宋文国
Owner RUNTAI CHEM TAIXING CO LTD