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Green synthesis method for benzoin

A technology of green synthesis and benzoin, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of low catalytic efficiency, large dosage, and difficulty in catalyst synthesis, and achieve simple process and rich sources of raw materials Effect

Active Publication Date: 2014-08-27
HUANGSHAN HUAHUI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solve the problems of difficult catalyst synthesis, large dosage, low catalytic efficiency and high production cost in the synthesis of benzoin in the industry

Method used

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  • Green synthesis method for benzoin

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Effect test

Embodiment 1

[0022] The synthesis of embodiment 1 imidazole hydrochloride

[0023] Add 68g of imidazole into the four-necked flask, dissolve it in 100ml of tetrahydrofuran, slowly add 85ml of 37% hydrochloric acid solution dropwise to the flask through the dropping funnel, keep the reaction temperature at 60-70°C, and put it into an ice-water bath to crystallize after reacting for 1h. Filtrate and dry to obtain imidazole hydrochloride, and obtain 98.6 g of imidazole hydrochloride with a yield of about 95%.

Embodiment 2-1

[0024] The synthesis of embodiment 2-1 benzoin

[0025] Add 106g of raw materials benzaldehyde, 1.0g of imidazole hydrochloride, 72g of absolute ethanol, a buffer solution of sodium dihydrogen phosphate and disodium hydrogen phosphate in a certain ratio, adjust the pH value to 7.8-8.5, and react at 80°C 2h. Put it into an ice-water bath for crystallization and filtration to obtain a light yellow benzoin solid, which was washed with a small amount of ethanol to obtain white needle-shaped crystals and dried under normal pressure to obtain 98.8 g of the finished product.

Embodiment 3

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Abstract

The invention discloses a green synthesis method for benzoin. The green synthesis method includes the steps of firstly, putting benzaldehyde and imidazole hydrochloride into a reaction kettle according to the molar ratio ranging from 1:0.003 to 1:0.015, adding absolute ethyl alcohol solvents accounting for, by mass, 60% to 75% of the benzaldehyde, adjusting the pH value of the reaction system to range from 7.8 to 8.5, and conducting reaction for 1.5 hours to 2.5 hours at the temperature ranging from 70 DEG C to 90 DEG C; secondly, after the reaction ends, placing the reaction kettle in the ice-water bath to be processed through crystallization and filtering, obtaining crystallization mother liquor and light yellow solid, washing the light yellow solid through alcohol to obtain white acicular crystals, and conducting drying under the normal pressure to obtain the finished product, namely, the benzoin. By means of the method, traditional virulent editpotassium cyanide catalysts or sodium cyanide catalysts are replaced, and therefore the new green chemical synthesis method capable of reducing by-products is achieved. The method solves the problems that at present, catalysts obtained through synthesis in the industry are high in toxicity or low in toxicity but difficult to synthetise, high in consumption, low in catalysis efficiency and high in production cost.

Description

technical field [0001] The invention relates to a green synthesis method of benzoin. Background technique [0002] Benzoin, also known as benzoin, has a chemical name of 1,2-diphenyl anhydrous ethanol ketone, which is a white needle-like crystal. As an important chemical raw material, benzoin is widely used as a photosensitizer for photosensitive resins, a dye intermediate, and an anti-cratering agent for powder coatings. Synthesis of ureides and preparation of diphenylethylenedione, diphenylethylenedione oxime, acetic acid benzoin compounds, etc. [0003] The traditional synthetic method of benzoin is to use benzaldehyde in hot absolute ethanol solution with potassium cyanide or sodium cyanide as a catalyst. This method has a high yield and is easy to operate. The only defect is that the catalyst is a highly toxic chemical , It is more troublesome in the storage and recovery of the catalyst. There are huge risks not only in production but also in safety, and wastewater t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/83C07C45/75B01J31/02
CPCB01J31/0244B01J2231/342C07C45/75C07C49/83
Inventor 方向宏冯乙巳杨志萍汤增荣何领曹镇汪鹏飞
Owner HUANGSHAN HUAHUI TECH
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