Process fof hydrogenating carboxylic acid and its ester to prepare alcohol

A technology of ester hydrogenation and carboxylic acid, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of high reaction pressure and high temperature, achieve mild reaction conditions, simplified separation or purification process, Highly active and selective effect

Inactive Publication Date: 2007-06-06
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalytic system still has the problems of high reaction pressure (8MPa) and high temperature (230-300°C)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 30 parts of RuCl 2 (TPPTS) 3 The aqueous solution was heated to 50°C in a constant temperature water bath, and 41 parts of ammonia solution and 29 parts of zirconium oxychloride aqueous solution were added dropwise to the three-necked bottle at the same time. , after vacuum drying, Ru / ZrO 2 catalyst. Add 26 parts of methyl propionate, 73 parts of water into a stirred autoclave, and then add 1 part of Ru / ZrO 2 The catalyst was replaced 3 times with high-purity hydrogen, filled with hydrogen at a pressure of 5.0 MPa, and reacted for 10 hours at a temperature of 150°C. After cooling, the reaction solution was taken out to obtain 26 parts of n-propanol. The product composition was analyzed by gas chromatography. The results showed that, The conversion rate of methyl propionate was 99.5%, and the selectivity of n-propanol was 99.5%.

Embodiment 2

[0033] 30 parts of RhCl 2 (TPPTS) 3 The aqueous solution was heated to 45°C in a constant temperature water bath, and 41 parts of ammonia solution and 29 parts of zirconium oxychloride aqueous solution were added dropwise to the three-necked bottle at the same time. , and dried under vacuum to obtain Rh / ZrO 2 catalyst. Add 92 parts of methyl propionate and 5 parts of water to a stirred autoclave, followed by 3 parts of Rh / ZrO 2 The catalyst was replaced 4 times with high-purity hydrogen, filled with hydrogen at a pressure of 5.0 MPa, and reacted for 10 hours at a temperature of 150 ° C. After cooling, the reaction solution was taken out to obtain 77 parts of n-propanol. The product composition was analyzed by gas chromatography. The results showed that, The conversion rate of methyl propionate was 90.0%, and the selectivity of n-propanol was 92.5%.

Embodiment 3

[0035] 24 parts of RuCl2 (TPPTS) 3 The aqueous solution and 12 parts of tin chloride aqueous solution are heated to 55 °C in a constant temperature water bath, and 23 parts of ammonia solution and 41 parts of zirconium oxychloride aqueous solution are added dropwise to the three-necked bottle at the same time. After the drop is complete, precipitation occurs and continue to stir overnight, the precipitate was filtered off and dried in vacuo to give RuSn / ZrO 2 catalyst. Add 50 parts of ethyl lactate and 40 parts of water to a stirred autoclave, followed by 10 parts of RuSn / ZrO 2 The catalyst was replaced 5 times with high-purity hydrogen, charged with hydrogen at a pressure of 5.0 MPa, and reacted for 12 hours at a temperature of 150°C. After cooling, the reaction solution was taken out to obtain 50 parts of 1,2-propanediol. The product composition was analyzed by gas chromatography. The results showed that the conversion rate of ethyl lactate was 99%, and the selectivity of ...

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PUM

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Abstract

The present invention discloses process of preparing alcohol with carboxylic acid and its ester, and features that C2-C20 carboxylic acid and its ester in 21-92 weight portions, catalyst in 1-21 weight portions and solvent in 5-73 weight portions are added into reactor and reacted with high purity hydrogen at the temperature of 100-200 deg.c, preferably 100-150 deg.c and pressure not lower than 1.0 MPa, preferably 3.0-7.0MP a while stirring at 500-1000 rpm for 6-24 hr to produce alcohol, with the alcohol being taken out after cooling. The carboxylic acid and its ester may have straight chain or branched chain, and the catalyst is solid in the carrier of zirconia in precipitation process sol or marketable product. Gas chromatographic analysis shows the present invention has the conversion rate of carboxylic acid and its ester in 75.0-99.5 % and selectivity of 68.2-99.5 %.

Description

technical field [0001] The invention relates to a method for preparing alcohol by hydrogenation of carboxylic acid and its ester, which belongs to the field of organic synthesis and catalytic reaction. Background technique [0002] Alcohol, the product of the hydrogenation reaction of carboxylic acids and their esters, has high application value, and it is widely used in pharmaceutical intermediates and organic synthesis. In addition, fatty acids and their esters are important components of animal and vegetable oils, and have a wide range of sources , low price. This reaction generally uses Group VIII metals or their compounds as catalysts. Catalysts such as copper chromium or copper zinc chromium were the first catalysts used in the hydrogenation reaction of carboxylic acids and their esters, but these catalysts often require high temperature (>200°C) and pressure (20-30MPa) for hydrogenation. . Later, precious metals such as ruthenium and rhodium were used as catalys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/149C07C31/02B01J23/46B01J23/62B01J23/89
Inventor 李瑞祥李贤均樊光银
Owner SICHUAN UNIV
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