Production method of cyclohexanone ketal perfume for daily cosmetics

A cyclohexanone ketal and production method technology, which is applied in the field of daily chemicals, can solve the problems of reduced catalytic activity, strong inorganic acid corrosion, and many side reactions, and achieves less catalyst consumption, improved dispersion, improved activity and stability Effect

Inactive Publication Date: 2021-05-11
王强
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the defects of severe inorganic strong acid corrosion, serious environmental pollution and many side reactions in the traditional production process of cyclohexanone ketal compounds, the present invention proposes a green catalyst for producing cyclohexanone ketal compounds and its Preparation method to solid superacid SO 4 2- / SnO 2 -TiO 2 Combined with acidic ionic liquid
The prepared catalyst can not only solve the defect that the catalytic activity is greatly reduced due to the easy loss of acidity, but also can largely inhibit the catalyst from corroding the reaction equipment and the occurrence of side reactions

Method used

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  • Production method of cyclohexanone ketal perfume for daily cosmetics

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of preparation method that is used to produce the catalyst of cyclohexanone-1,3-butanediol ketal, is to realize by following specific steps:

[0029] (1) Mesoporous SnO 2 -TiO 2 preparation of

[0030] Dissolve titanyl sulfate, tin tetrachloride and CTAC in deionized water respectively, stir at room temperature for 15 min, then add urea to the above mixed solution and continue to stir for 15 min, then place the resulting mixture in a water bath at 90 °C Stirring treatment for 18h, the resulting product was filtered and washed to no Cl - After drying at 105°C for 16h, the obtained product was roasted at 550°C for 5h to obtain SnO 2 -TiO 2; The addition of the CTAC is 4wt% of the total weight of zirconyl chloride; the concentration of titanyl sulfate in the above mixed solution is 0.2mol / L; the concentration of substance of tin tetrachloride is 0.4mol / L ; The addition of urea is 20 times the amount of the total substance of titanyl sulfate and tin tetrachlorid...

Embodiment 2

[0040] A kind of preparation method that is used to produce the catalyst of cyclohexanone-1,3-butanediol ketal, is to realize by following specific steps:

[0041] (1) Mesoporous SnO 2 -TiO 2 preparation of

[0042] Dissolve titanyl sulfate, tin tetrachloride and CTAC in deionized water respectively, stir at room temperature for 15 min, then add urea to the above mixed solution and continue to stir for 15 min, then place the resulting mixture in a water bath at 90 °C Stirring treatment for 20h, the resulting product was filtered and washed to no Cl - After drying at 105°C for 16h, the obtained product was roasted at 550°C for 5h to obtain SnO 2 -TiO 2 ; The addition of the CTAC is 5wt% of the total weight of zirconyl chloride; the concentration of titanyl sulfate in the above mixed solution is 0.2mol / L; the concentration of substance of tin tetrachloride is 0.2mol / L ; The addition of urea is 20 times the amount of the total substance of titanyl sulfate and tin tetrachlori...

Embodiment 3

[0052] A kind of preparation method that is used to produce the catalyst of cyclohexanone-1,3-butanediol ketal, is to realize by following specific steps:

[0053] (1) Mesoporous SnO 2 -TiO 2 preparation of

[0054] Dissolve titanyl sulfate, tin tetrachloride and CTAC in deionized water respectively, stir at room temperature for 15 min, then add urea to the above mixed solution and continue to stir for 15 min, then place the resulting mixture in a water bath at 90 °C Stirring treatment for 24h, the resulting product was filtered and washed to no Cl - After drying at 105°C for 16h, the obtained product was roasted at 550°C for 5h to obtain SnO 2 -TiO 2 ; The addition of the CTAC is 6wt% of the total weight of zirconyl chloride; the concentration of titanyl sulfate in the above mixed solution is 0.4mol / L; the concentration of substance of tin tetrachloride is 0.2mol / L ; The addition of urea is 20 times the amount of the total substance of titanyl sulfate and tin tetrachlori...

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Abstract

The invention discloses a production method of cyclohexanone ketal perfume for daily cosmetics. The method comprises the following steps: uniformly mixing cyclohexanone, 1, 3-butanediol and a catalyst, adding the mixture into a reaction kettle, centrifugally separating out the catalyst after the reaction is finished, sequentially washing the obtained organic phase with water and saturated salt water until the organic phase is neutral, and drying the anhydrous magnesium sulfate, and then carrying out refined vacuum distillation operation to obtain a cyclohexanone-1, 3-butanediol ketal finished product. The catalyst is formed by combining solid superacid SO4 < 2-> / SnO2-TiO2 and an acidic ionic liquid, wherein the mass fraction of the solid superacid in the catalyst is 70wt%-85wt%, and concretely by preparing mesoporous SnO2-TiO2, preparing solid superacid SO4 < 2-> / SnO2-TiO2, and compounding the solid superacid SO4 < 2-> / SnO2-TiO2 and an acidic ionic liquid. The catalyst prepared by the invention not only can overcome the defect that the catalytic activity is greatly reduced due to easy loss of acidity, but also can inhibit corrosion of the catalyst to reaction equipment and the occurrence of side reaction to a great extent.

Description

technical field [0001] The invention belongs to the technical field of daily chemicals, and relates to a production technology of fragrances for daily cosmetics, in particular to a production method of cyclohexanone ketal fragrances for daily cosmetics. Background technique [0002] Spices are composed of natural spices and synthetic spices. Synthetic spices have been widely used in Japan due to their stable quality, low price fluctuations, and production not restricted by climate, natural environment, and geographical conditions, thus ensuring stable supply. Used in cosmetics, skin care products and food and other fields. Because natural spice plants are often limited by natural conditions and factors such as processing, the number of varieties and product quality are affected to a certain extent. Because synthetic spices are not restricted by natural conditions, the quality is stable, the scale of production can be arranged by people themselves, and the price of the produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/08B01J31/02B01J27/053A61K8/49
CPCA61K8/498A61K2800/10B01J23/002B01J27/053B01J31/0282C07D319/08
Inventor 王强
Owner 王强
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