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A kind of method for catalyzed synthesis of cyclohexanone ethylene glycol ketal by titanium ammonium phosphotungstate compound salt

A cyclohexanone glycol ketal, titanium phosphotungstate technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problem of repeated use performance It can avoid the increase of by-products, have excellent catalytic performance, and promote efficient synthesis.

Active Publication Date: 2021-03-30
SHAOYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned single-type heteropolyacid salt catalysts still have defects such as low activity and selectivity, or poor reusability.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Catalyst preparation: Weigh 0.25 mmol of ammonium carbonate, 0.5 mmol of titanium sulfate and 1 mmol of phosphotungstic acid and dissolve them in 20 ml of deionized water; after dissolving, slowly add the titanium sulfate solution dropwise to In the phosphotungstic acid solution, react for 0.5 hours, then slowly add ammonium carbonate solution dropwise, and gradually form a white precipitate; after the dropwise addition, continue to stir and react for 0.5 hours, let stand and age for 1 hour, the precipitate is separated by filtration, dried, The molecular formula can be obtained as (NH 4 ) 0.5 Ti 0.5 h 0.5 PW 12 o 40 ammonium titanium phosphotungstate compound salt.

Embodiment 2

[0024] The preparation of catalyst: preparation process is the same as embodiment 1, only the add-on of ammonium carbonate is changed into 0.2 mmol, the add-on of titanium sulfate is changed into 0.6 mmol, molecular formula can be obtained as (NH 4 ) 0.4 Ti 0.6 h 0.2 PW 12 o 40 ammonium titanium phosphotungstate compound salt.

Embodiment 3

[0026] The preparation of catalyst: preparation process is the same as embodiment 1, only the add-on of ammonium carbonate is changed into 0.3 mmol, the add-on of titanium sulfate is changed into 0.4 mmol, molecular formula can be obtained as (NH 4 ) 0.6 Ti 0.4 h 0.8 PW 12 o 40 ammonium titanium phosphotungstate compound salt.

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Abstract

The invention relates to a method for catalytic synthesis of cyclohexanone ethylene ketal from titanium phosphotungstate and ammonium phosphotungstate composite salt. The titanium phosphotungstate andammonium phosphotungstate composite salt is taken as a catalyst, cyclohexanone ethylene ketal is generated from cyclohexanone and ethylene glycol through a condensation reaction, and the condensed structural formula of the titanium phosphotungstate and ammonium phosphotungstate composite salt is (NH4)xTiyH(3-x-4y)PW12O40, wherein x=0.4-0.6, and y=0.4-0.6. The titanium phosphotungstate and ammonium phosphotungstate composite salt as the catalyst has larger specific surface area, higher surface acid density and proper acid strength, so that the catalyst has excellent catalytic performance, andproduct yield is high. Besides, raw materials of the catalyst are easily available, the preparation process is simple, the catalyst and the product are easy to separate, and the catalyst is recyclable.

Description

technical field [0001] The invention relates to a method for synthesizing cyclohexanone ethylene glycol ketal, in particular to a method for catalyzing the synthesis of cyclohexanone ethylene glycol ketal by titanium ammonium phosphotungstate compound salt, which belongs to the field of organic synthesis. Background technique [0002] Cyclohexanone ethylene glycol ketal is a transparent liquid with a slight smell of bitter almonds. It has the fragrance of flowers, trees and mint, and the fragrance is soft and has good fragrance-fixing effect. middle. [0003] In the traditional production process of cyclohexanone ethylene glycol ketal, liquid acids such as concentrated sulfuric acid, hydrochloric acid and phosphoric acid are mainly used as catalysts, and the catalysts are cheap and have high catalytic activity. However, there are many by-products in the reaction, and it is difficult to separate and purify the products. In addition, liquid acids such as sulfuric acid severe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/72B01J31/18B01J27/188
CPCB01J27/188B01J27/24C07D317/72Y02P20/584
Inventor 张振华张超
Owner SHAOYANG UNIV
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