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
View PDF4 Cites 3 Cited by
  • 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 h

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0024] Example 1: Preparation of cyclohexanone glycol ketal

[0025] In a 50 mL three-necked flask were added 4.9 g (0.05 mol) of cyclohexanone, 0.07 mol of ethylene glycol, 10 g of cyclohexane with water agent and 0.2450 g (5%) of catalyst fly ash. Install a thermometer, a water separator and a reflux condenser, place it in a heating mantle, heat to reflux for 3h, cool to room temperature, filter the liquid in the reaction flask to recover fly ash, combine it with the liquid in the water separator, and wash with distilled water three times , After drying with anhydrous sodium sulfate, remove the solvent to obtain the crude product, distill under reduced pressure, collect the distillate, weigh and calculate the yield to reach 93%. 1 HNMR(500MHz, CDCl 3 )δ 1.57 (m, 3H), 1.77 (m, 2H), 3.88 (s, 4H).

Example Embodiment

[0028] Example 2: Preparation of cyclohexanone glycol ketal

[0029] In a 50 mL three-necked flask, 4.9 g (0.05 mol) of cyclohexanone, 0.07 mol of ethylene glycol, 10 g of cyclohexane with water agent and 0.049 g (1%) of catalyst fly ash were added. Install a thermometer, a water separator and a reflux condenser, place it in a heating mantle, heat to reflux for 3h, cool to room temperature, filter the liquid in the reaction flask to recover fly ash, combine it with the liquid in the water separator, and wash with distilled water three times , After drying with anhydrous sodium sulfate, remove the solvent to obtain the crude product, distill under reduced pressure, collect the distillate, weigh and calculate the yield to reach 54%.

Example Embodiment

[0030] Example 3: Preparation of cyclohexanone glycol ketal

[0031] In a 50mL three-necked flask, 4.9g (0.05mol) of cyclohexanone, 0.07mol of ethylene glycol, 10g of cyclohexane with water agent and 0.3g (6%) of catalyst fly ash were added. Install a thermometer, a water separator and a reflux condenser, place it in a heating mantle, heat to reflux for 3h, cool to room temperature, filter the liquid in the reaction flask to recover fly ash, combine it with the liquid in the water separator, and wash with distilled water three times , After drying with anhydrous sodium sulfate, remove the solvent to obtain the crude product, distill under reduced pressure, collect the distillate, weigh and calculate the yield to reach 91%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap