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A kind of method for preparing pseudoionone

A technique for pseudo-ionone and acetone, which is applied in the field of preparing pseudo-ionone, can solve the problems of low yield, high toxicity and corrosiveness of the reaction solution and the like

Active Publication Date: 2022-01-07
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the catalyst is easy to obtain and the production cost is not high in this process, the reaction solution is highly toxic and corrosive, and the treatment of spent caustic soda after use has also attracted much attention; meanwhile, the yield of this method is not high, generally between 60% and 80%.

Method used

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  • A kind of method for preparing pseudoionone
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The preparation of embodiment 1 catalyst

[0039] Will K 2 HPO 4 (5.60g) and KH 2 PO 4 (0.41g) mixed, slowly added 9994.00g of deionized water to dilute, stirred for 1h until uniformly mixed, and obtained a phosphate catalyst solution. Its composition is: K 2 HPO 4 0.056wt%, KH 2 PO 4 0.0041wt%, H 2 O99.94wt%; pH7.8.

[0040] Embodiment 2 citral condensation reaction

[0041] Add citral (0.1mol, 15.22g), acetone (0.5mol, 29.04g), 4.91g of the phosphate catalyst solution prepared in Example 1 into a 250.0mL three-necked flask, double row pipe nitrogen replacement protection, stir with a magnet , turn on the condensate water, reflux the condensing tube, heat up to 60.0°C of the reaction solution, reflux the condensing tube for 3 hours, and maintain normal pressure during the reaction. After the reaction was completed, the temperature was lowered and the liquid was separated to obtain the reaction product. The reaction products were qualitatively analyzed by ...

Embodiment 10

[0046] Embodiment 10 Catalyst recovery applies mechanically

Embodiment 2

[0047] In Example 2, the reaction solution was poured into the separatory funnel and left to stand for 30min, separated and reclaimed the lower floor water phase catalyst, the pH of the reclaimed phosphate catalyst solution was 7.2, adding K 2 HPO 4 Adjust the pH to 7.8 to obtain a phosphate catalyst solution.

[0048] Add citral (0.1mol, 15.22g), acetone (0.5mol, 29.04g), and 4.91g of the above-mentioned phosphate catalyst solution into a 250.0mL three-necked flask, protect it by nitrogen replacement with a double row tube, stir with a magnet, and open the condensed water , the condensing tube was refluxed, the temperature was raised to 60.0° C. of the reaction liquid, the condensing tube was refluxed for 3 hours, and normal pressure was maintained during the reaction. After the reaction was completed, the temperature was lowered and the liquid was separated to obtain the reaction product. The reaction products were qualitatively analyzed by chromatography-mass spectrometer...

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Abstract

The invention discloses a method for preparing pseudoionone. The method uses phosphate as a catalyst to prepare pseudo-ionone by a liquid-liquid two-phase method, can inhibit the self-polymerization of citral, improve catalytic selectivity, has high catalyst activity, can be recycled, and is environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and relates to a method for preparing pseudoionone. Background technique [0002] Pseudo-ionone can be synthesized by Aldol condensation of citral separated from litsea cubeba oil and acetone in the presence of sodium hydroxide solution as a catalyst. Pseudo-ionone is an important intermediate for the synthesis of flavors and fragrances such as ionone, vitamins A, E and β-carotene. Commonly used condensation catalysts are strong alkaline aqueous solutions such as NaOH / KOH. Although these catalysts can make the yield reach about 85%, they have disadvantages such as long reaction time and complicated post-treatment process, which are unfavorable for reducing production costs and continuous production. Moreover, after the reaction, the lye catalyst is difficult to separate from the reactant, and the too strong alkalinity makes the raw material citral easy to self-polymerize, resulting in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/74C07C45/80C07C47/21B01J27/18
CPCC07C45/74C07C45/80B01J27/1806C07C47/21Y02P20/584
Inventor 朱龙龙张涛吕英东郭劲资张旭程晓波王延斌林龙翟文超李莉宋军伟杨宗龙黎源
Owner WANHUA CHEM GRP CO LTD
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