Unlock instant, AI-driven research and patent intelligence for your innovation.

Palladium carbon catalyst for α-alkylation reaction of ketone and alcohol and preparation method thereof

A palladium-carbon catalyst and an alkylation reaction technology are applied in the preparation of hydroxyl compounds, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of low selectivity, unsuitable catalysts, and low catalytic activity, and achieve catalytic activity. High, good research and industrial application prospects, the effect of simple process

Active Publication Date: 2018-06-05
JIANGXI HANS PRECIOUS METALS CO LTD +1
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a palladium-carbon catalyst for the α-alkylation reaction of ketones and alcohols and a preparation method thereof. Low selectivity, low catalytic activity, the catalyst can not be used mechanically and other problems, provides a method to improve the catalytic activity of palladium carbon catalyst, so that the alkylation reaction is more thorough, the target product selectivity and the advantages of good stability in recycling

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Palladium carbon catalyst for α-alkylation reaction of ketone and alcohol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Step 1. Heat and stir the activated carbon with 1mol / L hydrochloric acid at 50°C for 4 hours, then wash it with deionized water until neutral, and dry it at 110°C to obtain activated carbon as a carrier;

[0018] Step 2, adjust the pH value of palladium chloride solution to 5 with sodium carbonate, then mix with the gac obtained in step 1;

[0019] Step 3: Heat and stir the slurry in Step 2 at 80° C. for 2 hours, keep it warm and reduce it with a formaldehyde reducing agent to obtain a palladium-carbon catalyst.

Embodiment 2

[0021] Get 10g of the palladium-carbon catalyst prepared in Example 1 to prepare a slurry, slowly add 1mL of 5mmol / L sodium borohydride alkaline solution (0.5% NaOH), continue to stir for 12h, filter, wash until neutral, and vacuum at 80°C After drying, the hydrophobic palladium carbon catalyst is obtained.

Embodiment 3

[0023] Take 10 g of the palladium-carbon catalyst prepared in Example 1 and prepare it into a slurry, slowly add 3 mL of 5 mmol / L sodium borohydride alkaline solution (0.5% NaOH), continue to stir for 12 h, filter, wash until neutral, and dissolve the mixture at a temperature of 80 ° C. Vacuum-dried to obtain a hydrophobic palladium-carbon catalyst.

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 relates to a preparation method of a palladium-charcoal catalyst for an alpha-alkylation reaction of ketone and alcohol and a preparation method thereof. The preparation method comprises the following steps: acidifying and washing a carrier; adsorbing a palladium salt component: dissolving palladium salt with sodium carbonate to adjust the pH value to 5 and then mixing the solution with activated charcoal slurry; reducing: reducing palladium hydroxide adsorbed on the activated charcoal to metal palladium; washing the metal palladium with deionized water to be neutral and removing chloride ions to obtain a palladium-charcoal catalyst precursor product; and performing surface hydrophobic treatment on the palladium-charcoal catalyst, treating the palladium-charcoal catalyst precursor product in a sodium borohydride alkaline solution for a certain time, and washing the solution to be neutral to obtain a hydrophobic palladium-charcoal catalyst. According to the catalyst provided by the invention is used for the alpha-alkylation reaction of ketone and alcohol, and generation of a byproduct, namely coupled alcohol, is reduced.

Description

technical field [0001] The invention belongs to the technical field of preparation of noble metal catalysts, and in particular relates to a palladium-carbon catalyst for the α-alkylation reaction of ketones and alcohols and a preparation method thereof. Background technique [0002] The coupling reaction of ketones and alcohols is an important pathway for C-C bond formation. It has been widely concerned for a long time, and transition metal-catalyzed alcohols as alkylating reagents are the focus of chemists from all over the world in the research of organic synthesis. Compared with the traditional alkylation method (which usually needs to be carried out under low temperature and anhydrous conditions), the by-product of this method is only water, the reaction operation is simple, and the conditions are mild. It is a green and environmentally friendly method. At present, it is necessary to find some realization A method for preparing coupling ketone compounds by catalyzing th...

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
Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07C29/38C07C33/20
CPCB01J23/44C07C29/38C07C33/20
Inventor 卢新宁李阳明高艳妮郁丰善汤港华李永敏何治鸿相亚波程龙
Owner JIANGXI HANS PRECIOUS METALS CO LTD