Method for preparing benzalacetone

A technology for benzylidene acetone and acetone, which is applied in the field of preparing benzylidene acetone, can solve the problems of many by-products, high production cost, seriousness and the like, and achieves the effects of mild reaction conditions, simple preparation method, and easy separation and recovery.

Inactive Publication Date: 2020-02-21
JIANGXI HUAYU AROMATIC TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the process is mature and the yield is stable, this method has a large amount of wastewater discharge, serious pollution, and the catalyst cannot be reused.
At present, most of the preparation methods of benzylidene acetone focus on the development and research of new catalysts, such as some potassium fluoride/alumina catalysts, polyvinyl chloride polyvinyl polyamine resin catalysts, tributylamine aminated strong basic anion exchange Resin catalysts, etc., have al

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The catalyst used in the preparation of benzylidene acetone is CaO-MgO loaded with potassium carbonate.

[0019] The preparation process of the CaO-MgO of loaded potassium carbonate is:

[0020] Control the molar ratio of magnesium chloride and calcium chloride to 7:1, add an excess of 20wt% sodium hydroxide solution dropwise to the aqueous solution of magnesium chloride and calcium chloride at a temperature of 50°C, stir and react for 2.5 hours, then let it stand for 5 hours , the product was filtered, washed with deionized water, and dried at 105°C to obtain a solid CaO-MgO product; at room temperature, the solid CaO-MgO was soaked in a saturated solution of potassium carbonate for 6 hours, and then filtered and Dry and then calcinate at 550° C. for 3 h to obtain a CaO-MgO catalyst loaded with potassium carbonate.

Embodiment 2

[0022] The present invention uses acetone and benzaldehyde as raw materials, CaO-MgO loaded with potassium carbonate as a catalyst, dibutyl hydroxytoluene as a polymerization inhibitor, and obtains benzylidene acetone through aldol condensation, specifically comprising the following steps:

[0023] Step 1: Aldol Condensation

[0024] Put acetone, CaO-MgO loaded with potassium carbonate, and xylene into the reaction kettle, add benzaldehyde dropwise at a temperature of 35°C, and then carry out aldol condensation at 45°C for 3.5 hours, and the content of benzaldehyde in the product is ≤1wt% end the reaction;

[0025] Wherein the molar ratio of benzaldehyde and acetone is 1:2, the amount of CaO-MgO loaded with potassium carbonate is 7% of the acetone mass, the mass ratio of xylene and benzaldehyde is 1:1, and the amount of inhibitor dibutyl hydroxytoluene 1‰ of the mass of benzaldehyde;

[0026] Step 2: Wash

[0027] The reaction product of step 1 was allowed to stand for 30 m...

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PUM

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Abstract

The invention provides a method for preparing benzalacetone. According to the method, acetone and benzaldehyde are used as raw materials, CaO-MgO loaded with potassium carbonate is used as a catalyst,butylated hydroxytoluene is used as a polymerization inhibitor, and aldol condensation is conducted to obtain benzalacetone; product yield and product purity reach 91% or above and 99% or above respectively; and in the preparation process, the molar ratio of benzaldehyde to acetone is 1: (1.7-2.1), the usage amount of CaO-MgO loaded with potassium carbonate accounts for 5%-10% of the mass of acetone, the usage amount of the polymerization inhibitor butylated hydroxytoluene accounts for 0.1%-0.3% of the mass of benzaldehyde, and a molar ratio of magnesium chloride to calcium chloride is (6-8):1. The preparation method is simple, has the characteristics of mild reaction conditions, easy separation and recovery of the catalyst, high product yield, few byproducts and the like, and can easilyrealize industrial production.

Description

technical field [0001] The invention relates to a method for preparing benzylidene acetone, which specifically belongs to the technical field of organic synthesis. Background technique [0002] The molecular structure of benzylidene acetone contains functional groups such as phenyl, alkenyl, and carbonyl, and has active reactivity. It is an important intermediate for the synthesis of medicines, pesticides, and spices. The method for synthesizing benzylidene acetone in industry is generally to produce the target product through the Claisen condensation of benzaldehyde and acetone under the action of dilute alkali. Although this method has a mature process and stable yield, it has a large amount of wastewater discharge, serious pollution, and the catalyst cannot be reused. At present, most of the preparation methods of benzylidene acetone focus on the development and research of new catalysts, such as some potassium fluoride / alumina catalysts, polyvinyl chloride polyvinyl pol...

Claims

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Application Information

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IPC IPC(8): C07C49/217C07C45/74B01J27/232
CPCB01J27/232C07C45/74C07C49/217
Inventor 俞忠华章志福余喜彪全怨青
Owner JIANGXI HUAYU AROMATIC TECH
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