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Method for catalytic synthesis of pseudo ionone through solid super base

A technology of pseudoionone and solid super base, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, carbon-based compounds, etc., can solve the problems of high toxicity and corrosion, low yield, etc. Easy to prepare, high catalytic activity and selectivity

Inactive Publication Date: 2019-01-11
朱晓萍
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this step has brought some highly toxic and corrosive properties, and the treatment of spent caustic soda after use has attracted much attention; meanwhile, the productive rate of this method is not high, generally at 60-80%

Method used

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  • Method for catalytic synthesis of pseudo ionone through solid super base

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Preparation of super strong solid base:

[0031] Add 14.8g of magnesium nitrate and 10.65g of zirconium nitrate to 30mL of water and 100mL of ethanol to make a solution, add 1mol / L LiOH to the solution, the pH value is 11, reflux and aging for 36 hours, centrifuge, the precipitate is washed with water, dried overnight, in nitrogen Under the atmosphere, the precipitate was put into a muffle furnace and calcined at a high temperature of 800° C. for 3 hours to obtain a solid superbase catalyst A with a Li content of 2%.

[0032] 2) Add 1 mol of citral, 1 mol of acetone, and 0.05 mol of the solid superbase catalyst A prepared above into the reactor, under the protection of nitrogen, the reaction temperature is 150°C for aldol condensation reaction for 3 hours, and the normal pressure is maintained during the reaction. After the reaction is finished, cool down and filter to take the filtrate, add acetic acid dropwise for neutralization, wash with water to remove the aceti...

Embodiment 2

[0034] 1) Preparation of super strong solid base:

[0035] Add 14.8g of magnesium nitrate and 8.52g of zirconium nitrate to 30mL of water and 100mL of ethanol to make a solution, add 1mol / L LiOH to the solution, the pH value is 11, reflux and aging for 36 hours, centrifuge, the precipitate is washed with water, dried overnight, in nitrogen Under the atmosphere, the precipitate was put into a muffle furnace and calcined at a high temperature of 800° C. for 3 hours to obtain a solid superbase catalyst B with a Li content of 0.7%.

[0036] 2) Add 1 mol of citral, 3 mol of acetone, and 0.05 mol of the solid superbase catalyst B prepared above into the reactor, and under the protection of nitrogen, the reaction temperature is 150°C for aldol condensation reaction for 3 hours, and normal pressure is maintained during the reaction. After the reaction is finished, cool down and filter to take the filtrate and add acetic acid dropwise for neutralization, then wash with water to remove ...

Embodiment 3

[0038] 1) Preparation of super strong solid base:

[0039] Add 14.8g of magnesium nitrate and 10.65g of zirconium nitrate to 30mL of water and 100mL of ethanol to make a solution, add 1mol / L LiOH to the solution, the pH value is 10, reflux and aging for 36 hours, centrifuge, the precipitate is washed with water, dried overnight, in nitrogen Under the atmosphere, the precipitate was put into a muffle furnace and calcined at a high temperature of 800° C. for 3 hours to obtain a solid superbase catalyst C with a Li content of 1.1%.

[0040] 2) Add 1 mol of citral, 1 mol of acetone, and 0.1 mol of the solid superbase catalyst C prepared above into the reactor, under the protection of nitrogen, the reaction temperature is 150°C for aldol condensation reaction for 3 hours, and the normal pressure is maintained during the reaction. After the reaction is finished, cool down and filter to take the filtrate, add acetic acid dropwise for neutralization, wash with water to remove the acetic...

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Abstract

The invention relates to a method for catalytic synthesis of pseudo ionone through solid super base. By compounding an oxide, namely solid super base, the catalytic activity and selectivity of a catalyst are high, the auto-agglutination problem of raw materials, namely citral and acetone caused by a common catalyst is solved, the use amount is low, and the preparation is simple, convenient and feasible; and the catalyst has no possibility of corroding a reactor, belongs to an environment-friendly catalyst and can be centrifugally separated after the reaction is finished, so that repeated use can be realized.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a method for catalyzing the synthesis of pseudoionones by a solid superbase. Background technique [0002] Pseudo-ionone, chemical name 6,10-dimethyl-undecatrien-2-one, molecular formula C 13 h 20 O, with a molecular weight of 192.3, is a light yellow liquid with a boiling point of 114-116°C (2mmHg). It is an important intermediate in the synthesis of flavors and fragrances such as ionone, vitamins A, E and β-carotene. It is used in flavors and fragrances, medicines, food additives and It is widely used in synthetic chemistry. [0003] For a long time, domestic and foreign scholars have been continuously improving the research on the synthesis process. Its main synthetic method is obtained by condensing citral separated from litsea cubeba oil with acetone through Aldol under alkaline conditions. Therefore, it is very important to master its alkaline conditions and temperature con...

Claims

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Application Information

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IPC IPC(8): C07C45/74C07C49/203
CPCC07C45/74C07C49/203
Inventor 朱晓萍
Owner 朱晓萍
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