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Method of preparing terpinyl acetate

A technology of terpineol acetate and terpineol, applied in the field of preparation of terpineol acetate, can solve the problems of difficult regeneration of solid superacid, complicated preparation process, low service life, etc., and achieves low cost, simple preparation method, and easy use. long life effect

Inactive Publication Date: 2008-09-24
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation process of solid superacid with multi-component carrier is complicated, the cost is high, and its service life is still not high, such as SO 4 2- / SnO 2 -TiO 2 After the catalyst was used 5 times, the conversion rate of terpineol changed from 98.6% when used for the first time to 88.7%
Moreover, the regeneration of solid superacid is difficult, and it needs to be impregnated again with corresponding acid such as sulfuric acid, and roasted at high temperature to activate regeneration.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] First prepare 200 ml of sulfuric acid solution with a concentration of 0.06 mol / L, and then divide this solution into two equal parts. Add aniline monomer in wherein a part of acidic solution, form the aniline solution that concentration is 0.16mol / L, add ammonium persulfate in another part of acidic solution, form ammonium persulfate solution, the molar concentration of said aniline solution and The molar concentration ratio of the ammonium persulfate solution was 1.0. Then quickly pour the ammonium persulfate solution into the aniline solution at room temperature, and stir vigorously for 4.5 hours, then wash with distilled water and ethanol three times in turn, and vacuum-dry the obtained blue-black solid powder at 65°C for 12 hours , to obtain nanometer polyaniline solid acid catalyst. Under the action of polyaniline solid acid catalyst doped with sulfuric acid, chemically pure terpineol and analytically pure acetic anhydride are used as raw materials to esterify te...

Embodiment 2

[0021] First prepare 200 ml of hydrochloric acid solution with a concentration of 0.7 mol / L, and then divide this solution into two equal parts. Add aniline monomer in wherein a part of acidic solution, form the aniline solution that concentration is 0.36mol / L, add ammonium persulfate in another part of acidic solution, form ammonium persulfate solution, the molar concentration of said aniline solution is the same as The molar concentration ratio of the ammonium persulfate solution was 1.2. Then quickly pour the ammonium persulfate solution into the aniline solution at room temperature, and stir vigorously for 5 hours, then wash with distilled water and ethanol for 4 times, and dry the resulting blue-black solid powder in vacuum at 70°C for 10 hours , to obtain nanometer polyaniline solid acid catalyst. Under the action of polyaniline solid acid catalyst doped with hydrochloric acid, chemically pure terpineol and analytically pure acetic anhydride are used as raw materials to...

Embodiment 3

[0023] First prepare 200 ml of nitric acid solution with a concentration of 0.9 mol / L, and then divide this solution into two equal parts. Add aniline monomer in wherein a part of acidic solution, form the aniline solution that concentration is 0.8mol / L, add ammonium persulfate in another part of acidic solution, form ammonium persulfate solution, the molar concentration of said aniline solution is the same as The molar concentration ratio of the ammonium persulfate solution was 0.8. Then quickly pour the ammonium persulfate solution into the aniline solution at room temperature, and stir vigorously for 8 hours, then wash with distilled water and ethanol for 4 times, and dry the resulting blue-black solid powder in vacuum at 80°C for 6 hours , to obtain nanometer polyaniline solid acid catalyst. Under the action of polyaniline solid acid catalyst doped with nitric acid, chemically pure terpineol and analytically pure acetic anhydride are used as raw materials to esterify terp...

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Abstract

The present invention provides a preparation method of terpinyl acetate. The method is characterized in that the acid solution of one of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid and hydriodic acid is divided into two portions; aniline monomer and ammonium persulfate are respectively added; then aniline monomer solution and ammonium persulfate solution can be prepared. The aniline monomer solution and the ammonium persulfate solution are mixed rapidly and treated through a series of processes to prepare the nano polyaniline solid-acid catalyst. The prepared catalyst is used for the esterification of terpinyl and acetic anhydride to prepare the terpinyl acetate. The nano polyaniline catalyst doped with acid and prepared in the method has the advantages of simple preparation, low cost, and higher catalytic activity and selectivity in the esterification of the terpinyl and the acetic anhydride so as to prepare the terpinyl acetate (the transformation ratio of the terpinyl reaches to more than 95 percent, and the yield of the terpinyl acetate reaches to more than 80 percent). At the same time, the catalyst has the characteristics of easy separation and long service life.

Description

technical field [0001] The invention relates to a preparation method of terpineol acetate, in particular to a method for preparing terpineol acetate by using terpineol and acetic anhydride as raw materials under the action of a nano polyaniline solid acid catalyst, and belongs to the field of preparation of terpineol acetate. Background technique [0002] Terpine acetate has a distinct lemon and lavender aroma, and is widely used as a modifier and main fragrance in food, cosmetics and medicines. The current industrial synthesis method uses phosphoric acid as a catalyst to obtain it through the esterification reaction of terpineol and acetic anhydride. This method has the disadvantages of long synthesis time (16 hours), the catalyst cannot be recovered, it needs to consume a lot of water washing, pollute the environment, corrode equipment, etc., so its application is more and more limited. In recent years, many researchers hope to replace phosphoric acid with solid acid. If...

Claims

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Application Information

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IPC IPC(8): C07C69/12C07C67/08B01J31/06
Inventor 贾庆明王亚明陕绍云
Owner KUNMING UNIV OF SCI & TECH
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