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Method for synthesizing crotyl alcohol by converting ethanol through photocatalysis

A technology of crotyl alcohol and photocatalysis, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve the problems of undiscovered photocatalytic ethanol, etc., achieve environmental friendliness, mild reaction conditions, and simple synthesis process Effect

Active Publication Date: 2018-03-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] No photocatalytic ethanol conversion method to synthesize crotyl alcohol was found after searching

Method used

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  • Method for synthesizing crotyl alcohol by converting ethanol through photocatalysis
  • Method for synthesizing crotyl alcohol by converting ethanol through photocatalysis

Examples

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Embodiment 1

[0033] 10mmol Cd(NO 3 ) 2 4H 2 O and 30mmol thiourea (CN 2 h 4 S) respectively dissolved in 60mL of ethylenediamine, fully dissolved and mixed evenly, then placed in a 100mL high-pressure homogeneous reactor, heated at a rate of 5°C / min, and kept at 160°C for 48h. Centrifuge and wash to neutral, and place overnight in a vacuum oven at 60°C. One-dimensional CdS solid powder can be obtained after drying and grinding. Then add the prepared 0.2g CdS powder into 30mL dissolved with 0.025g Ni(NO 3 ) 2 ·6H 2 O, 0.025g sodium molybdate (NaMo 2 o 4 2H 2 O) and 0.06g of cysteine ​​(L-cysteine) in the aqueous solution, fully dispersed, placed in a 60ml high-pressure homogeneous reactor, heated at a rate of 5°C / min, and kept at 200°C for 24h. Centrifuge and wash several times, and place in a vacuum oven at 60°C overnight to obtain a 12wt%-NiMoS@CdS photocatalyst. Take 5mg of the prepared 12wt%-NiMoS@CdS photocatalyst and add it to 20mL of 1M NaOH ethanol solution, pass inert g...

Embodiment 2

[0035] 10mmol Cd(NO 3 ) 2 4H 2 O and 30mmol thiourea (CN 2 h 4S) respectively dissolved in 60mL of ethylenediamine, fully dissolved and mixed evenly, then placed in a 100mL high-pressure homogeneous reactor, heated at a rate of 5°C / min, and kept at 160°C for 48h. Centrifuge and wash to neutral, and place overnight in a vacuum oven at 60°C. One-dimensional CdS solid powder can be obtained after drying and grinding. Add the prepared 0.2g CdS powder to 30mL and dissolve 0.02g sodium molybdate (Na 2 MO 6 ) and 0.05g of cysteine ​​(L-cysteine) in an aqueous solution, fully dispersed, placed in a 60ml high-pressure homogeneous reactor, heated at a rate of 5°C / min, and kept at 200°C for 12h. Centrifuged and washed several times, placed in a vacuum oven at 60°C overnight to obtain 12wt%-MoS 2 / CdS photocatalyst. Take 2mg of the prepared 12wt%-MoS 2 The @CdS photocatalyst was added to 50mL of 1M KOH ethanol solution, and the inert gas argon was introduced under stirring to fu...

Embodiment 3

[0037] 10mmol Cd(NO 3 ) 2 4H 2 O and 30mmol thiourea (CN 2 h 4 S) respectively dissolved in 60mL of ethylenediamine, fully dissolved and mixed evenly, then placed in a 100mL high-pressure homogeneous reactor, heated at a rate of 5°C / min, and kept at 160°C for 48h. Centrifuge and wash to neutral, and place overnight in a vacuum oven at 60°C. One-dimensional CdS solid powder can be obtained after drying and grinding. Then add 0.2g of the prepared CdS powder into 50mL lactic acid aqueous solution (30wt%), after fully dispersed, add chloroplatinic acid solution according to the loading capacity of 1wt%, stir and blow nitrogen. Reduction with a 200W xenon lamp for 3h yielded CdS loaded with Pt nanoparticles. Centrifuge and wash several times, and place overnight in a vacuum oven at 60°C for later use. Take 5mg of the prepared 1wt%-Pt@CdS photocatalyst and add it to 20mL 0.01M NaOH ethanol solution. After stirring, pass inert gas argon to fully replace the oxygen in the syste...

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Abstract

The invention relates to a method for synthesizing crotyl alcohol by converting ethanol through photocatalysis. The method comprises the steps of adding a semiconductor photocatalyst for modifying a cocatalyst into an ethanol solution of alkali; after magnetically feeding nitrogen for fully replacing oxygen in a system, starting an ultraviolet light source or a visible light source for reacting for 1 to 200h, and converting the ethanol into the crotyl alcohol; after separating the catalyst from a solution, separating the crotyl alcohol from the raw material ethanol to obtain the crotyl alcohol. The method provided by the invention has the advantages that the raw materials are cheap and easy to get, a technological process is simple, the conversion rate is high, and the selectivity is good.

Description

technical field [0001] The invention belongs to a chemical synthesis method, in particular to a photocatalytic ethanol conversion synthesis method for crotyl alcohol. Background technique [0002] The proposal of photocatalytic organic synthesis has opened up a new synthetic route. It has attracted great attention due to its use of renewable solar energy as a light source and its ability to achieve chemical reactions that cannot be achieved by conventional thermochemistry under mild conditions. Photocatalytic organic synthesis is usually carried out at normal temperature and pressure, is easy to operate, and generally does not produce secondary pollution. Although there are reasons such as low reaction conversion rate and poor product selectivity, no photocatalytic synthesis technology has been industrialized so far. C-C coupling is the core of organic synthesis. Applying semiconductor photocatalysis to C-C coupling to prepare high-value compounds is a promising organic sy...

Claims

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Application Information

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IPC IPC(8): C07C29/34C07C33/03
CPCC07C29/34C07C33/03
Inventor 陈加藏晁玉广郑剑锋张海霞王志坚李娜贾素萍李莉张莉朱珍平
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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