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

Active Publication Date: 2022-03-25
陈军民
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the ketene-acetone condensation conversion method is the main industrial synthesis method at present. Only one company in Japan adopts the "ethyl acetoate and ketene method", and the rest use the "ketene-acetone condensation conversion method", but the method is changed. There are still obvious disadvantages of high energy consumption and low yield
The problems existing in our country's existing technology are: 1. The one-way conversion rate of acetone cracking is low, the carbonization loss is serious, and the waste heat is not recycled.
2. The absorption rate of vinegar is low, and the vinegar is not complete
3. In the separation process of the vinegar liquid, deacidify first, and then recover acetone. The process of obtaining intermediates from the kettle liquid is unreasonable, the separation performance of the tower is not good, the capacity is insufficient, and the loss is too much
4. The separation and purification tower of acetylacetone has insufficient equipment capacity, insufficient separation performance, and unclear operating temperature control area. 5. The single-pass conversion rate of isomerization is low, the carbonization loss is serious, and the content of high boiling substances and impurities is too high
[0003] In terms of the utilization rate of carbon atoms, the isomerization of isopropenyl acetate to synthesize acetylacetone is the most reasonable, but the single-pass conversion rate in the isomerization process is difficult to control, and there are many impurities. The development of a suitable catalyst can greatly optimize the isomerization. structure process, thereby improving the yield and purity of acetylacetone

Method used

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  • A kind of acetylacetone synthesis catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

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

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/85C07C49/14C07C45/54C07C45/78
CPCC07C45/54C07C45/78B01J29/85C07C49/14
Inventor 林伯祥谢伟朱云飞陈永明施国敏
Owner 陈军民
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