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Catalyst for preparing n-Butyl butyrate by n-butanal and preparation method thereof

A technology of n-butyl n-butyrate and n-butyraldehyde is applied in catalyst activation/preparation, aldehyde redox preparation, chemical instruments and methods, etc. Highly selective effect

Active Publication Date: 2018-02-02
TIANJIN BOHUA YONGLI CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is aimed at the difficulty of immobilizing Ru ions. The catalyst is based on Porous Organic Polymer (POP), a porous organic polymer rich in hydroxyl groups. The POP in this patent is different from other literatures in that it contains hydroxyl groups and forms Ru on its surface. Complex structure (structural formula 1), is a new type of porous organic catalyst

Method used

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  • Catalyst for preparing n-Butyl butyrate by n-butanal and preparation method thereof
  • Catalyst for preparing n-Butyl butyrate by n-butanal and preparation method thereof
  • Catalyst for preparing n-Butyl butyrate by n-butanal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 50g of 1,2-dichloroethane into the flask as a solvent, add 2g of phenol, 5g of dimethoxymethane, add 2g of ferric chloride under vigorous stirring, heat to 80°C, phenol and dimethyl Oxymethane is homogeneously polymerized under the action of ferric chloride, and the polymerization time is 12h. Soxhlet extraction was performed on the obtained solid with ethanol as a solvent for 18 hours to obtain a hydroxyl-rich porous organic polymer material POP. The obtained porous organic polymer material was dispersed in toluene, 3.6 g of tert-butyllithium was added, and stirred at room temperature for 4 h. The polymer POP-Li was obtained by suction filtration. The obtained POP-Li was redispersed in toluene, 5g of ruthenium trichloride was added, heated to 80°C, stirred for 4 hours, and the polymer POP-Ru was obtained by suction filtration.

Embodiment 2

[0034] Add 25g of 1,2-dichloroethane into the flask as a solvent, add 2g of phenol and 5g of dimethoxymethane, add 1g of ferric chloride under vigorous stirring, and heat to 85°C to make phenol and dimethoxymethane Methoxymethane is homogeneously polymerized under the action of ferric chloride, and the polymerization time is 20h. The obtained solid was subjected to Soxhlet extraction with ethanol as a solvent for 12 hours. A hydroxyl-rich porous organic polymer material POP was obtained. The obtained porous organic polymer material was dispersed in toluene, 3.6 g of n-butyllithium was added, and stirred at room temperature for 5 h. The polymer POP-Li was obtained by suction filtration. The obtained POP-Li was redispersed in cyclohexane, 5 g of ruthenium acetylacetonate was added, heated to 60° C., stirred for 7 h, and the polymer POP-Ru was obtained by suction filtration.

Embodiment 3

[0036] Add 50g of 1,2-dichloroethane into the flask as a solvent, add 2g of phenol and 6g of dimethoxymethane, add 0.5g of ferric chloride under vigorous stirring, heat to 90°C, phenol and dimethoxymethane Methoxymethane is homogeneously polymerized under the action of ferric chloride, and the polymerization time is 24h. The obtained solid was subjected to Soxhlet extraction with ethanol as a solvent for 24 hours. A hydroxyl-rich porous organic polymer material POP was obtained. The obtained porous organic polymer material was dispersed in toluene, 4.2 g of tert-butyllithium was added, and stirred at room temperature for 6 h. The polymer POP-Li was obtained by suction filtration. The obtained POP-Li was redispersed in toluene, 6g of ruthenium nitrate was added, heated to 100°C, stirred for 6h, and the polymer POP-Ru was obtained by suction filtration.

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PUM

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Abstract

The invention relates to a catalyst for preparing n-Butyl butyrate by n-butanal and a preparation method thereof. The catalyst is prepared by the following steps: using a hydroxy-enriched porous organic polymer as a substrate, and forming a complexation structure of Ru on the surface of the substrate; firstly preparing a hydroxy-enriched porous organic polymer material POP; adding tert-butyl lithium or n-butyl lithium, and preparing a polymer POP-Li; and adding ruthenium salt to obtain a polymer POP-Ru. The catalyst has the characteristics of good stability, repeated use, and higher reaction conversion rate and selectivity. The preparation method is capable of creatively fixing Ru ions on the surface of the catalyst, a new idea is provided for the preparation of the catalyst, and the catalyst has the significant application value.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a catalyst for preparing n-butyl n-butyrate from n-butyraldehyde and a preparation method thereof. Background technique [0002] Butyl butyrate is a colorless or light yellow transparent oily liquid, which is a kind of butyrate esters. Butyl butyrate is an edible spice that is allowed to be used in my country's "National Food Safety Standard Food Additive Use Standard" (GB 2760-2014). It is often used to prepare banana, pineapple, apple and other fruity flavors and whiskey flavors. It is widely used as an additive for candy, biscuits, soft drinks, bread, ice cream and other foods for the flavoring of cream essence. Butyl butyrate is also used as a solvent in nitrocellulose, shellac, coumarone resins and paints. With the continuous improvement of the downstream market of butyl butyrate, various new uses are being effectively developed. Among them, butyl butyrate...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J37/30C07C67/44C07C69/24
CPCB01J31/1691B01J37/30B01J2531/0213B01J2531/821C07C67/44C07C69/24
Inventor 庞栓林高进王义龙杜文强李云辉侯磊磊王海石松王松刘宇娜张波李越苗淳
Owner TIANJIN BOHUA YONGLI CHEM IND
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