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Method for preparing cyclohexanone glycol ketal compounds by directly using fly ash as catalyst

A cyclohexanone diol ketal and compound technology, which is applied in the field of organic compound preparation, can solve the problems of ignoring the application potential of fly ash, and achieve the effects of easy industrial production, high yield, and broad application prospects

Active Publication Date: 2016-08-03
山东鑫泰化工产业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, although environmental protection scientists and researchers have devoted themselves to the development and research of the environmental protection utilization of fly ash, they have neglected the application potential of the special structure of fly ash itself as a cheap catalyst, and there are few direct applications of fly ash as a catalyst Reports in Organic Reactions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: the preparation of cyclohexanone ethylene glycol ketal

[0025] Add 4.9g (0.05mol) of cyclohexanone, 0.07mol of ethylene glycol, 10g of water-carrying agent cyclohexane and 0.2450g (5%) of catalyst fly ash in a 50mL three-necked flask. Install a thermometer, a water separator and a reflux condenser, place it in a heating jacket, heat to reflux for 3 hours, cool to room temperature, filter the liquid in the reaction bottle to recover fly ash, combine it with the liquid in the water separator, and wash it three times with distilled water , after drying over anhydrous sodium sulfate, the solvent was removed to obtain a crude product, which was distilled under reduced pressure, and fractions were collected, and the yield by weighing was 93%. 1 HNMR (500MHz, CDCl 3 )δ1.57(m,3H),1.77(m,2H),3.88(s,4H).

Embodiment 2

[0028] Embodiment 2: the preparation of cyclohexanone ethylene glycol ketal

[0029] Add 4.9g (0.05mol) of cyclohexanone, 0.07mol of ethylene glycol, 10g of water-carrying agent cyclohexane and 0.049g (1%) of catalyst fly ash in a 50mL three-necked flask. Install a thermometer, a water separator and a reflux condenser, place it in a heating jacket, heat to reflux for 3 hours, cool to room temperature, filter the liquid in the reaction bottle to recover fly ash, combine it with the liquid in the water separator, and wash it three times with distilled water , after drying over anhydrous sodium sulfate, the solvent was removed to obtain a crude product, which was distilled under reduced pressure, collected fractions, and the yield was calculated to reach 54%.

Embodiment 3

[0030] Embodiment 3: the preparation of cyclohexanone ethylene glycol ketal

[0031] Add 4.9g (0.05mol) of cyclohexanone, 0.07mol of ethylene glycol, 10g of water-carrying agent cyclohexane and 0.3g (6%) of catalyst fly ash in a 50mL three-necked flask. Install a thermometer, a water separator and a reflux condenser, place it in a heating jacket, heat to reflux for 3 hours, cool to room temperature, filter the liquid in the reaction bottle to recover fly ash, combine it with the liquid in the water separator, and wash it three times with distilled water , after drying over anhydrous sodium sulfate, the solvent was removed to obtain a crude product, which was distilled under reduced pressure, and fractions were collected, and the yield by weighing was 91%.

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Abstract

The invention discloses a method for preparing cyclohexanone glycol ketal compounds. The method is characterized in that fly ash is directly used as a catalyst to catalyze the condensation dehydration reaction of cyclohexanone compounds and glycol compounds to obtain the cyclohexanone glycol ketal compounds. The fly ash is directly used as the catalyst for synthesizing cyclohexanon eglycol ketal through the condensation of clohexanone and glycol without any treatment; the fly ash is cheap and easily available; the problem that solid catalysts are difficult to industrialize due to low cost performance and the environmental problems brought by the fly ash are solved to some extent; compared with the prior art in which an ammonium persulfate-modified fly ash catalyst is used, the method has the advantage that the yield is higher when fly ash is directly as a catalyst for catalyzing the condensation dehydration reaction of 4-tert-butyl cyclohexanone or cyclohexandione and the glycol compounds.

Description

technical field [0001] The invention belongs to the technical field of organic compound preparation, and relates to a method for catalytically preparing organic compounds with a novel catalyst, and more specifically, to a method for directly using fly ash to catalyze and prepare cyclohexanonediol ketal compounds. Background technique [0002] Ketal (aldehyde) compounds are a class of high-grade new flavors that have developed rapidly in the past two decades. They have a better fragrance than their parent compounds and are widely used in daily flavors and food flavors. In addition, in organic synthesis, the protection of carbonyl compounds into ketal (aldehyde) intermediates is also a particularly important organic synthesis strategy, and has particularly broad applications in multi-step organic synthesis. The cyclohexanone ethylene glycol ketal compound is one of the ketal fragrances. It has floral and mint fragrance and has a good fragrance-fixing effect. Cyclohexanone eth...

Claims

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Application Information

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IPC IPC(8): B01J23/78C07D317/72
CPCB01J23/78C07D317/72
Inventor 郑祖彪韩冰冰郝加龙吴方刘杰张勇程玲
Owner 山东鑫泰化工产业技术研究院有限公司
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