A kind of acetylacetone synthesis catalyst and preparation method thereof

A technology of acetylacetone and catalyst, applied in the field of acetylacetone synthesis catalyst and preparation thereof, can solve the problems of high content of high boilers and impurities, insufficient separation performance, poor separation performance, etc., and achieves improved yield and purity, significant economical effect of benefit

A technology of acetylacetone and catalyst, applied in the field of acetylacetone synthesis catalyst and preparation thereof, can solve the problems of high content of high boilers and impurities, insufficient separation performance, poor separation performance, etc., and achieves improved yield and purity, significant economical effect of benefit

CN109675618BActive Publication Date: 2022-03-25陈军民

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  • A kind of acetylacetone synthesis catalyst and preparation method thereof

Examples

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Embodiment 1

[0022] A kind of acetylacetone synthesis catalyst and preparation method thereof, comprising the following steps:

[0023] (1) Take 10 parts of expanded perlite and a specific surface area of ​​250 m 2 / g SAPO-11 molecular sieve 30 parts were mixed, 1.5 parts of 20% dilute sulfuric acid and 10 parts of deionized water were added, heated to 80 °C, stirred for 30 min, and calcined at 250-400 °C to obtain a catalyst carrier;

[0024] (2) Grind and pulverize 0.5 part of manganese oxide and 0.3 part of cobalt oxide, pass through a 10-mesh sieve, add it to the chlorinated hydrocarbon impregnation solution in proportion, and stir for 10 minutes to obtain an impregnation solution;

[0025] (3) The catalyst carrier was impregnated with the impregnation solution for 24 hours, dried at 110 °C for 4 hours, and calcined at 350-500 °C to obtain the catalyst;

Embodiment 2

[0027] A kind of acetylacetone synthesis catalyst and preparation method thereof, comprising the following steps:

[0028] (1) Take 10 parts of expanded perlite and a specific surface area of ​​280 m 2 Mix 30 parts of SAPO-11 molecular sieve / g, add 1 part of 20% dilute sulfuric acid and 5 parts of deionized water, heat to 80°C, stir for 30min, and roast at 250-400°C to obtain a catalyst carrier;

[0029] (2) Grind and pulverize 0.5 part of manganese oxide and 0.5 part of cobalt oxide, pass through a 10-mesh sieve, add to the chlorinated hydrocarbon impregnation solution in proportion, and stir for 10 minutes to obtain an impregnation solution;

[0030] (3) The catalyst carrier was impregnated with the impregnation solution for 24 hours, dried at 110 °C for 4 hours, and calcined at 350-500 °C to obtain the catalyst;

Embodiment 3

[0032] A kind of acetylacetone synthesis catalyst and preparation method thereof, comprising the following steps:

[0033] (1) Take 10 parts of activated carbon and a specific surface area of ​​260 m 2 / g 20 parts of SAPO-11 molecular sieves were mixed, 1.5 parts of 20% dilute sulfuric acid and 10 parts of deionized water were added, heated to 80 °C, stirred for 30 min, and calcined at 250-400 °C to obtain a catalyst carrier;

[0034] (2) Grind and pulverize 0.5 part of manganese oxide and 1 part of nickel oxide, pass through a 10-mesh sieve, add to the chlorinated hydrocarbon impregnation solution in proportion, and stir for 10 minutes to obtain an impregnation solution;

[0035] (3) The catalyst carrier was impregnated with the impregnation solution for 24 hours, dried at 110 °C for 4 hours, and calcined at 350-500 °C to obtain the catalyst;

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Abstract

The present invention relates to the technical field of organic synthesis, in particular to an acetylacetone synthesis catalyst and a preparation method thereof, comprising the following components in parts by weight: 10 parts of inorganic carrier materials, 0.5-2 parts of manganese oxide, 0.3-1 part of iron-based element oxidation Thing, 10-30 parts SAPO-11 molecular sieves. The preparation method comprises the following steps: mixing the inorganic carrier material and SAPO-11 molecular sieve in proportion, adding dilute sulfuric acid and deionized water, heating to 80°C and stirring for 30 minutes, and roasting at 250-400°C to obtain the catalyst carrier; manganese oxide and iron Grinding and pulverizing element oxides, adding them to the impregnating solution in proportion, stirring for 10-15min to obtain the impregnating solution; impregnating the catalyst carrier with the impregnating solution for 24-48h, drying at 110°C for 4h, and roasting at 350-500°C Get a catalyst. The catalyst obtained by the invention is used in the isomerization process of isopropenyl acetate, which can effectively improve the conversion rate of isomerization, thereby improving the yield and purity of acetylacetone.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to catalyst technology, in particular to an acetylacetone synthesis catalyst and a preparation method thereof. Background technique [0002] Acetylacetone (2,4-pentanedione) is widely used, mainly used in the production of medicine, feed additives, petroleum cracking and hydrogenation catalysts, isomerization catalysts, synthetic material additives, surfactants, etc. At present, the production of acetylacetone mainly has two shortcomings of low yield and low product purity, which severely limits the development of its follow-up products. At present, the synthesis of acetylacetone has the following synthetic process routes. 1. Acetone-ethyl acetate method: Add metallic sodium, ether and cold anhydrous ethyl acetate into the reactor, add acetone dropwise with stirring, keep the reaction temperature at 45-55°C, and the optimum pH at 6-6.5. The reactants are separated and re...

Claims

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Application Information

Patent Timeline
25 Mar 2022
Publication
CN109675618B
IPC
B01J29/85; C07C49/14; C07C45/54; C07C45/78
CPC
C07C45/54; C07C45/78; B01J29/85; C07C49/14
Inventors
林伯祥; 谢伟