Method for preparing 4-heptanone from butanol

A technology of butanol and heptanone, which is applied in the field of ketoylation to prepare 4-heptanone, can solve the problems of poor activity, low yield of target product, cumbersome catalyst preparation, etc., and achieve the effect of simple preparation and high preparation efficiency

Active Publication Date: 2018-05-08
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

[0003] Although the research on the reaction route of preparing 4-heptanone from butanol has made some progress at present, the preparation of the catalyst is relatively cumbersome, or the catalyst has poor activity and the yield of the target product is low. A solid catalyst system with high reactivity and good stability is of great significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 25g of cerium nitrate hexahydrate and dissolve it in 2.5L of water, add ammonia water to adjust the pH=11, stir for 4h, filter, dry, and roast at 500°C for 4h to obtain 10g of cerium dioxide. The 14-25 mesh catalyst is taken from the forming screen and filled into the reaction tube, filled with a 5cm bed, and the mass space velocity of the raw material butanol is 0.5h -1 . The reaction was carried out at 400° C., and the chromatographic analysis was carried out every 2 hours. The conversion rate of butanol was 65%, and the selectivity of 4-heptanone was 88%.

Embodiment 2

[0029] Weigh 25g of cerium nitrate hexahydrate and dissolve it in 2.5L of water, add ammonia water to adjust the pH=11, stir for 4h, filter, dry, and roast at 500°C for 4h to obtain 10g of cerium dioxide. Forming sieve to take 14-25 mesh catalyst and fill it into the reaction tube, fill the 5cm bed layer, the quality of the raw material butanol is 1h -1 . The reaction was carried out at 400° C., and the chromatographic analysis was carried out every 2 hours. The conversion rate of butanol was 45%, and the selectivity of 4-heptanone was 85%.

Embodiment 3

[0031] Weigh 40g of cerium nitrate hexahydrate and dissolve it in 4L of water, add ammonia water to adjust the pH=11, stir for 4h, filter, dry, and roast at 500°C for 4h to obtain 16g of cerium dioxide. The 14-25 mesh catalyst is taken from the forming screen and filled into the reaction tube, filling the 8cm bed layer, and the mass space velocity of the raw material butanol is 1h -1 . The reaction was carried out at 420° C., and the chromatographic analysis was carried out every 2 hours. The conversion rate of butanol was 78%, and the selectivity of 4-heptanone was 83%.

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Abstract

The present invention relates to a method for preparing 4-heptanone from butanol, wherein specifically butanol is used as a raw material and is subjected to a reaction under a normal pressure with a catalyst cerium oxide or doped cerium oxide to obtain the product 4-heptanone, and the reaction device is a fixed-bed reactor. According to the present invention, cerium oxide or doped cerium oxide isused as the catalyst, and the catalyst is easily prepared, and can catalyze the high-selectivity generation of 4-heptanone, wherein the selectivity can reach more than 90%, and rge stability is good.

Description

technical field [0001] The invention relates to a method for preparing 4-heptanone, in particular to the preparation of 4-heptanone by ketolation with butanol as a reactant. Background technique [0002] 4-Heptanone is an important chemical raw material, which can be used as a solvent for nitrocellulose, as well as for the organic synthesis of food flavors and the preparation of flavors such as jackfruit, konker, bananas, and tropical fruits. 4-Heptanone is usually prepared from butyric acid by precipitation of calcium carbonate at 450 °C. Due to the wide range of sources of butanol, it can come from both petrochemical and biomass fermentation. Butanol is relatively active and can be oxidized or dehydrogenated to obtain butyric acid. Therefore, the direct preparation of 4-heptanone with butanol as a raw material has certain application prospects. In 2001, N.J.Coville et al. (N.D.Plint, N.J.Coville, D.Lack, G.L.Nattrass, T.Vallay.Journal of Molecular Catalysis A: Chemical,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/04C07C45/71
CPCC07C45/71C07C49/04
Inventor 王峰王业红张健张志鑫侯婷婷安静华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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