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Method for preparing pinacol by dehydrogenation of photocatalytic isopropanol dehydrogenation and hydrogenation coupling of acetone

A technology of isopropanol and photocatalysis, which is applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., to achieve the effects of single catalyst component, improved photocatalytic efficiency and good selectivity

Active Publication Date: 2013-03-20
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Some scholars also mentioned about the photochemical process of acetone in the presence of isopropanol solvent, the product has only a small amount of pinacol and 2,5-hexanedione, and a large amount of CO, CH 4 by-product formation

Method used

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  • Method for preparing pinacol by dehydrogenation of photocatalytic isopropanol dehydrogenation and hydrogenation coupling of acetone
  • Method for preparing pinacol by dehydrogenation of photocatalytic isopropanol dehydrogenation and hydrogenation coupling of acetone
  • Method for preparing pinacol by dehydrogenation of photocatalytic isopropanol dehydrogenation and hydrogenation coupling of acetone

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Experimental program
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Effect test

Embodiment 1

[0028] 1 g TiO 2 The photocatalyst was added to the 55.5 ml acetone-19.1 ml isopropanol-125.4 ml water reaction solution, argon gas was introduced under magnetic stirring, and after the air in the system was removed, a 300W high-pressure mercury lamp was turned on to carry out photocatalytic dehydrogenation of isopropanol and Acetone hydrogenation coupling reaction to prepare pinacol, reaction temperature 55 ℃, reaction time 36 h. After the reaction, the reaction solution was separated by static precipitation, and the solution was distilled to obtain the product pinacol. Chromatographic analysis showed that the conversion rate of acetone was 78.1%, the conversion rate of isopropanol was 63.8%, and the selectivity of pinacol was 91.2%.

Embodiment 2

[0030] After calcination at 600℃ for 8 h, 1 g TiO 2 The photocatalyst was added to the reaction solution of 18.5 ml acetone-19.1 ml isopropanol-120 ml water-42.4 ml cyclohexane, argon gas was introduced under magnetic stirring, and after the air in the system was removed, a 300 W high-pressure mercury lamp was turned on for photocatalyst Catalyze the coupling reaction of isopropanol dehydrogenation and acetone hydrogenation to prepare pinacol, the reaction temperature is 50℃, and the reaction time is 24 h. After the reaction, the reaction solution was separated by static precipitation. Chromatographic analysis showed that the conversion rate of acetone was 76.1%, the conversion rate of isopropanol was 52.8%, and the selectivity of pinacol was 83.4%.

Embodiment 3

[0032] Add 2.5 g of sodium tantalate photocatalyst prepared by hydrothermal method to 50 ml of acetone-50 ml of isopropanol-80 ml of water-20 ml of cyclohexane water reaction solution, and pass in argon gas under magnetic stirring to remove the After airing, a 500 W high-pressure mercury lamp was turned on to carry out the coupling reaction of photocatalytic isopropanol dehydrogenation and acetone hydrogenation to prepare pinacol. The reaction temperature was 45 °C and the reaction time was 180 h. After the reaction, the reaction solution was separated by static precipitation. Chromatographic analysis showed that the conversion rate of acetone was 93.5%, the conversion rate of isopropanol was 90.7%, and the selectivity of pinacol was 90.8%.

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Abstract

The invention discloses a method for preparing pinacol by dehydrogenation of photocatalytic isopropanol and hydrogenation coupling of acetone, comprising the following steps of: adding a semiconductor photocatalyst in a reaction solution which is composed of acetone, isopropanol and a solvent in a ratio of the reaction solution to the semiconductor photocatalyst of (100 to 500 ml): (0.1 to 3.5 g); magnetically stirring; illuminating at the inert atmosphere to react for 0.5-180 hours at the reaction temperature of 5-55 DEG C by dehydrogenation of photocatalytic isopropanol dehydrogenation and hydrogenation coupling of acetone; after the reaction is concluded, separating to obtain a catalyst and a solution; and distilling the solution to obtain the product, namely, pinacol. The method disclosed by the invention has the advantages of high conversion rate and good selectivity.

Description

technical field [0001] The invention relates to a photocatalytic synthesis method of pinacol, specifically a method for preparing pinacol by using a semiconductor photocatalyst to catalyze dehydrogenation of isopropanol and coupling hydrogenation of acetone under light conditions. Background technique [0002] Pinacol is also known as 2,3-dimethyl-2,3-butanediol; anhydrous pinacol; pinacol; tetramethylethylene glycol; Hydroxybutane, an important organic diol, is widely used in pesticide synthesis, rubber raw materials, organic synthesis and other fields, and is an important raw material for the synthesis of organic intermediates such as pinacolone and dimethylbutadiene. [0003] Pinacol is mainly synthesized by acetone reduction and tetramethylethylene glycolation. The method for preparing pinacol by reduction of acetone is to adopt magnesium amalgam, aluminum amalgam, sodium amalgam catalytic method or electrolytic method to prepare. The most commonly used method for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/38
Inventor 朱珍平曹宝月张健赵江红王志坚杨朋举
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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