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A kind of preparation method of solid heteropolyacid catalyst for synthesizing 1,8-cineole

A solid heteropolyacid and catalyst technology, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problem of liquid acid catalysts polluting the environment, 1,8- Solve the problems of low eucalyptol yield and large amount of liquid acid catalyst, and achieve the effects of easy operation, high selectivity and easy recovery

Active Publication Date: 2016-06-15
XIAMEN UNIV
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Problems solved by technology

[0006] However, the catalysts used in the above studies are mainly liquid acids such as inorganic acids or organic acids. The yield of 1,8-cineole obtained by the reaction is very low, the amount of liquid acid catalyst is large, and it is difficult to recycle, and the liquid acid catalyst has pollution to the environment and Severely corroded equipment and other problems

Method used

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  • A kind of preparation method of solid heteropolyacid catalyst for synthesizing 1,8-cineole
  • A kind of preparation method of solid heteropolyacid catalyst for synthesizing 1,8-cineole
  • A kind of preparation method of solid heteropolyacid catalyst for synthesizing 1,8-cineole

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Embodiment 1

[0028] Firstly, dry silica carrier is obtained by roasting in a muffle furnace according to the roasting procedure. The roasting procedure is: slowly increase the temperature at room temperature for 2 hours to 180°C (constant temperature for 1 hour); then slowly increase the temperature for 2 hours to 350°C (constant temperature for 1 hour); then slowly increase the temperature 2h to 550°C (6h constant temperature). According to the mass ratio of phosphotungstic acid to silica carrier 1:5, add phosphotungstic acid aqueous solution with a concentration of 0.0016g / ml, stir at a fixed speed for 12 hours, add ethanol according to the volume ratio of ethanol to phosphotungstic acid aqueous solution 2:1, and fix After stirring at a rotating speed, the solid filter cake was obtained by suction filtration. The filter cake was vacuum-dried at a drying temperature of 50°C and a vacuum of 0.08MPa for 48 hours, and then calcined at 200°C for 4 hours to obtain a phosphotungstic acid / silica...

Embodiment 2

[0030]First, according to the roasting procedure (see Example 1, the following examples are the same), roast in a muffle furnace to obtain a dry silica carrier, and add 0.0048g / ml concentration of phosphotungstic acid aqueous solution, after stirring at a fixed speed for 12 hours, add ethanol according to the volume ratio of ethanol and phosphotungstic acid aqueous solution at 2:1, stir at a fixed speed, and suction filter to obtain a solid filter cake. The filter cake was vacuum-dried at a drying temperature of 50°C and a vacuum of 0.08MPa for 48 hours, and then calcined at 200°C for 4 hours to obtain a phosphotungstic acid / silica solid heteropolyacid catalyst. Catalytic synthesis of 1,8-cineole is based on the mass ratio of raw material α-terpineol to solvent cyclohexane of 1:33.7, the mass ratio of catalyst to reaction solution of 0.0065:1, the reaction temperature is 60°C, and the reaction time is 5 hours. According to gas-mass chromatography analysis, the conversion rate ...

Embodiment 3

[0032] First, according to the roasting procedure (see Example 1, the following examples are the same), roast in a muffle furnace to obtain a dry silica carrier, and add 0.0032g / ml concentration of phosphotungstic acid aqueous solution, after stirring at a fixed speed for 12 hours, add ethanol according to the volume ratio of ethanol and phosphotungstic acid aqueous solution at 2:1, stir at a fixed speed, and suction filter to obtain a solid filter cake. The filter cake was vacuum-dried at a drying temperature of 50°C and a vacuum of 0.08MPa for 24 hours, and then calcined at 200°C for 4 hours to obtain a phosphotungstic acid / silica solid heteropolyacid catalyst. Catalytic synthesis of 1,8-cineole is based on the mass ratio of raw material α-terpineol to solvent cyclohexane of 1:33.7, the mass ratio of catalyst to reaction solution of 0.0065:1, the reaction temperature is 60°C, and the reaction time is 5 hours. GC-MS chromatographic analysis calculated that the conversion rate...

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Abstract

The invention discloses relates to 1,8-cineole and provides a preparation method for a solid heteropolyacid catalyst for synthesizing the 1,8-cineole. The solid heteropolyacid catalyst has the pollution-free, corrosion-free and reproducible effects and is high in catalysis activity and high in selectivity. The preparation method for the solid heteropolyacid catalyst comprises the steps of calcining a catalyst carrier; adding calcined catalyst carrier particles into a heteropolyacid aqueous solution, then adding ethyl alcohol, performing stirring and suction filtration to obtain a solid filter cake, and then drying and calcining the solid filter cake to obtain the solid heteropolyacid catalyst. A method for synthesizing the 1,8-cineole by catalyzing alpha-terpilenol by the solid heteropolyacid catalyst comprises the steps of adding the alpha-terpilenol and a solvent into a three-neck round-bottom flask, heating the flask to a pointed reaction temperature, adding the phosphotungstic acid / silicon dioxide catalyst to perform reaction, stopping heating-stirring when the pointed reaction time is achieved, cooling to the room temperature, and performing suction filtration and separation to obtain a reaction product.

Description

technical field [0001] The invention relates to 1,8-cineole, in particular to a method for preparing a solid heteropolyacid catalyst for synthesizing 1,8-cineole. Background technique [0002] 1,8-Cineole, the scientific name is 1,3,3-trimethyl-2-oxabicyclo[2,2,2]octane, is a kind of monoterpenoid compound with cool, spicy, Smell similar to camphor. Natural 1,8-cineole mainly exists in Eucalyptus eucalyptus of Myrtaceae plant and camphor tree of Lauraceae plant. It is an important fine chemical product and has been widely used in industrial fields such as food, daily chemical, medicine and catalyst preparation. (Li Shiyu, Wang Jingkang. A review of the application and preparation of eucalyptol [J]. Fine Chemical Industry, 1995,12(5):12). [0003] At present, natural extraction methods are used at home and abroad to prepare 1,8-cineole products. The main steps are: firstly use steam distillation to obtain the crude extract eucalyptus oil from the branches and leaves of Euca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/18B01J31/16C07D493/08
Inventor 王宏涛张东丽郑哲楠魏茹欣李军洪燕珍苏玉忠
Owner XIAMEN UNIV
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