Method for preparing esters through primary alcohol oxidation

A primary alcohol and oxygen technology, applied in the field of catalysts, can solve problems affecting the adsorption of substrates and intermediates, reduce selectivity, etc., and achieve the effects of easy separation, less by-products, and less dosage

Inactive Publication Date: 2015-09-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The generated water is more easily adsorbed on the hydrophilic catalyst carrier, which affects the adsorption of substrates and intermediates.
At the same time, the presence of water may also cause the further hydrolysis of the generated ester on the catalyst, reducing the selectivity

Method used

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  • Method for preparing esters through primary alcohol oxidation
  • Method for preparing esters through primary alcohol oxidation
  • Method for preparing esters through primary alcohol oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: Take 1.05g1wt%H by weighing 2 PtCl 6 ·H 2 O aqueous solution and 0.1 g of PVPK10 were dissolved in 40 mL of deionized water, then, 5 mL of 0.4 wt% NaBH was added under stirring condition 4 . Then 20mL was dispersed with 0.2g of hydrophobic carrier Ph-SiO 2 The ethanol solution was added to the above solution, stirred at room temperature for 12 hours, evaporated to dryness, washed with water for 3-5 times, and dried at 80°C for 12 hours. Catalyst named: 2wt%-Pt / Ph-SiO 2 (Based on Pt, the loading amount is 2wt%), the average size of Pt ions is 2.5nm, and the catalyst number is 1.

Embodiment 2

[0027] Embodiment 2: The preparation method of catalyst 2-20 adopts the method described in embodiment 1, just change different hydrophobic type supports, different metals and loading capacity, the metal source of Ru, Au, Pd is respectively RuCl 3 ·3H 2 O, HAuCl 4 4H 2 O, PdCl 2 , see Table 1 for details.

[0028] The preparation method of table 1 catalyst 2-20 and its properties

[0029]

Embodiment 3-20

[0030] Example 3-20: 0.2-2.0mmol 1-butanol, 0.002mmol (calculated as Pt) 2wt%-Pt / Ph-Ph-SiO 2 , 0.05mmol mesitylene (internal standard), 2mL solvent was added to a 30mL reaction kettle, the reaction kettle was sealed, air or oxygen at a certain pressure was introduced, and the temperature was raised to a certain temperature under stirring. After a certain period of reaction, cooled and centrifuged to separate the catalyst . The qualitative analysis of the obtained samples was performed by gas chromatography-mass spectrometry, and the quantitative analysis was realized by gas chromatography. The results are shown in Table 2.

[0031] Table 2 Oxidation of butanol to prepare butyl butyrate

[0032]

[0033] Analysis of the results in Table 2 shows that the hydrophobic carrier phenyl-modified silica (Ph-SiO 2 ) supported Pt catalyst 2wt%-Pt / Ph-SiO 2 , the best solvent for catalyzing molecular oxygen oxidation of n-butanol to butyl butyrate is toluene, the optimal condition is...

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Abstract

The invention relates to a method for preparing esters through primary alcohol oxidation. The method comprises the following steps: taking one or two of air and oxygen as an oxygen source, and oxidizing alcohols into esters under the catalytic action of hydrophobic carrier loaded metal nanoparticles. According to the method disclosed by the invention, the oxidation efficiency is high, and the product yield is high; the air or oxygen serves as an oxygen source, and the method is economic and environment-friendly; the product is separated from the catalyst, and the after-treatment is simple; and the catalyst is easily repeatedly used and has excellent application prospects.

Description

technical field [0001] The invention relates to a catalyst for preparing ester by oxidation of primary alcohol and its application. Background technique [0002] Esters are an important class of chemical raw materials, important intermediates in the synthesis of fine chemicals and bulk industrial chemicals, and are widely used in pharmaceuticals, spices, agricultural chemicals, polymers, etc. The traditional method is to dehydrate and esterify acid and its derivatives (acyl chloride, etc.) and alcohol under the action of acid catalyst. Commonly used acids, such as sulfuric acid, hydrochloric acid, etc., are corrosive. At the same time, the esterification reaction is a reversible reaction, and the presence of water makes the reaction incomplete, resulting in difficulties in separation. Using molecular oxygen as an oxidant to directly oxidize alcohols to esters in one step is a competitive new technology route, but it is also very challenging. At present, the catalysts used...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B41/12C07C67/40C07C69/24C07C69/614C07C69/612C07C69/65C07C69/734C07C69/618B01J31/02
Inventor 马继平徐杰贾秀全王敏石松高进苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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