Lewis acid catalyst as well as preparation method and application thereof in technique for producing acetylacetone by isopropenyl acetate displacement method

A technology of propylene acetate and Lewis acid is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of difficult separation and purification of products, high toxicity of lead-based catalysts, and easy environmental pollution. Achieve the effect of reducing the amount of carbonization and coking and the content of high-boiling by-products, improving production conditions and working environment, and improving product quality

Inactive Publication Date: 2009-07-22
HUZHOU XINAOTE PHARMA & CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of the preparation of acetylacetone by the isopropenyl acetate transposition method in the above process step three are: the lead catalyst used is highly toxic, easily pollutes the environment, the IPA reaction conversion rate is low, the carbonization loss is serious, the equipment is corroded, and the product is high. Excessive boiling content makes product separation and purification difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, a kind of Lewis acid composite metal transposition catalyst, is made up of aluminum trichloride, tin protochloride and sulfur, composition ratio is: aluminum trichloride: ethyl tin protochloride: sulfur element=80:50:20 . Its preparation method is:

[0020] 1. Anhydrous stannous chloride is dissolved in dehydrated ethanol of twice the amount under stirring for subsequent use;

[0021] 2. Add isopropenyl acetate in the reaction kettle, slowly add anhydrous aluminum trichloride under stirring, the feeding ratio (weight ratio) is, isopropenyl acetate: anhydrous aluminum trichloride=100:3, and control Temperature 60~70℃;

[0022] ③. Slowly add the material obtained in step ① into the reaction kettle of step ②, and control the temperature at 60-70°C;

[0023] ④. Then add sublimated sulfur into the above reaction kettle, stir for half an hour, cool down to below 50°C and discharge to get the catalyst product

[0024] The application method of the above-menti...

Embodiment 2

[0031] Embodiment 2. A Lewis acid composite metal transposition catalyst, which is composed of triethylaluminum, octyltin and sulfur, and the composition ratio is: triethylaluminum: octyltin: elemental sulfur = 20:5:1. Its preparation method is:

[0032] ①. Dissolve anhydrous octyltin in twice the amount of absolute ethanol under stirring;

[0033] ②. Add isopropenyl acetate in the reaction kettle, and slowly add anhydrous triethylaluminum under stirring. The feeding ratio (weight ratio) is: isopropenyl acetate:anhydrous triethylaluminum=100:3, and control Temperature 60~70℃;

[0034] ③. Slowly add the material obtained in step ① into the reaction kettle of step ②, and control the temperature at 60-70°C;

[0035] ④. Then add sublimated sulfur into the above reaction kettle, stir for half an hour, cool down to below 50°C and discharge to get the catalyst product

[0036] The application method of the above-mentioned Lewis acid composite metal transposition catalyst in the pr...

Embodiment 3

[0040] Embodiment 3, a kind of Lewis acid composite metal transposition catalyst, is made up of aluminum trichloride, iron salicylate and sulfur, composition ratio is: aluminum trichloride: iron salicylate: sulfur element=60:30:12 . Its preparation method is:

[0041] ①. Dissolve ferric salicylate anhydrous in three times the amount of absolute ethanol under stirring;

[0042] 2. Add isopropenyl acetate in the reaction kettle, slowly add anhydrous aluminum trichloride under stirring, the feeding ratio (weight ratio) is, isopropenyl acetate: anhydrous aluminum trichloride=100:3, and control Temperature 60~70℃;

[0043] ③. Slowly add the material obtained in step ① into the reaction kettle of step ②, and control the temperature at 60-70°C;

[0044] ④. Then add sublimated sulfur into the above reaction kettle, stir for half an hour, cool down to below 50°C and discharge to get the catalyst product

[0045] The application method of the above-mentioned Lewis acid composite met...

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PUM

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Abstract

The invention provides a Lewis acid catalyst, a preparation method and application thereof in a process for producing acetylacetone by an isopropenyl acetate dislocation method. The catalyst consists of a complex of aluminum, a complex of tin or a complex of iron and a sulfur element, wherein ratio of the complex of aluminum to the complex of tin or the complex of iron to the sulfur element is 80-20:50-5:20-1. The Lewis acid catalyst can be used for replacing the prior lead tetraethyl or tetramethyllead catalyst with stronger toxicity in a process for preparing the acetylacetone by the isopropenyl acetate dislocation method so as to improve production condition and working environment, improve reaction conversion rate of isopropenyl acetate to 4 to 10 percent, effectively reduce charring coke amount and content of a side product of a high-boiling product in the reaction, and improve quality of the product. The application of the catalyst does not adopt water as a reaction addition agent, so that decomposition of the isopropenyl acetate can be reduced.

Description

technical field [0001] The invention relates to a Lewis acid catalyst, in particular to a Lewis acid catalyst containing metal coordination complexes such as aluminum, tin and iron, and a preparation method and application thereof. Background technique [0002] Acetylacetone is an important chemical intermediate, mainly used in the chemical pharmaceutical industry, specifically for the synthesis of veterinary antibacterial drugs dysentery and sulfa drugs; it can also be used as a solvent for cellulose acetate, an additive for gasoline and lubricating oil, Synthetic solvent intermediates, metal ion extractants; metal complexes of acetylacetone are widely used as catalysts, etc. [0003] A kind of method that produces acetylacetone comparatively generally adopts at present is vinyl ketone-acetone method, and its process step is: one, adopt acetone or acetic acid to crack at high temperature to generate vinyl ketone; Two, absorb vinyl ketone with acetone to generate isopropenyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/14B01J31/12C07C49/14C07C45/54
Inventor 顾红高敏华林伯祥杨立新
Owner HUZHOU XINAOTE PHARMA & CHEM
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