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Preparation method of sodium ethoxide

A technology of sodium ethoxide and anhydrous ethanol is applied in the preparation of ethoxylation agents, the fields of strong basic catalysts in medicine and pesticide industry, and can solve the problems of high production cost, low yield, etc. The effect of simple process flow

Active Publication Date: 2016-02-03
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to overcome the problems such as low yield and high product

Method used

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  • Preparation method of sodium ethoxide

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Effect test

Embodiment 1

[0017] Add 100kg of sodium metal and 1kg of inhibitor to the reaction kettle, start stirring, open the vacuum valve, keep the vacuum at -0.01MPa, raise the temperature to 25°C, start adding 1000kg of absolute ethanol dropwise, control the dropping time for 2h, and control the temperature At 25-30°C; after the dropwise addition, continue to keep warm at 25-30°C for 2 hours. After the reaction, 1055kg of the product is obtained, with a yield of 95.91% and a content of 27.96%. It is a colorless viscous liquid.

Embodiment 2

[0019] Add 100kg of sodium metal and 3kg of inhibitors to the reaction kettle, start stirring, open the vacuum valve, keep the vacuum at -0.01MPa, cool down to 10°C, start adding 1200kg of absolute ethanol dropwise, control the dropping time for 3h, and control the temperature At 10-15°C; after the dropwise addition, continue to keep warm at 10-15°C for 2 hours. After the reaction, 1270kg of the product is obtained, the yield is 97.62%, the content is 23.23%, and it is a colorless viscous liquid.

Embodiment 3

[0021] Add 100kg of sodium metal and 5kg of inhibitors to the reaction kettle, start stirring, open the vacuum valve, keep the vacuum at -0.05MPa, raise the temperature to 30°C, start adding 1400kg of absolute ethanol dropwise, control the dropping time for 3h, and control the temperature At 15-25°C; after the dropwise addition, continue to keep warm at 15-25°C for 3 hours. After the reaction is completed, 1410kg of the product is obtained, with a yield of 94.01% and a content of 20.92%. It is a colorless viscous liquid.

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Abstract

The invention relates to a preparation method of sodium ethoxide. The preparation method comprises the following steps: adding metallic sodium and inhibitors to a reaction kettle at 0-30 DEG C, dropwise adding all absolute ethyl alcohol within 2-4 hours under the vacuum condition of minus 0.01-minus 0.05MPa and continuously reacting at 0-30 DEG C for 2-4 hours, thus obtaining sodium ethoxide with content more than 20% and yield more than 94%. The preparation method has the beneficial effects that the technological process is simple; little equipment, such as the reaction kettle and a condenser, are only used, so that the investment is low; reaction is carried out at a low temperature of 0-30 DEG C, thus reducing the consumption of condensate water and the energy consumption and saving the cost; meanwhile, the product has few impurities and good color and is a colorless and transparent viscous liquid; after the inhibitors are added, the storage time can be greatly lengthened under the low temperature and photophobic conditions and is more than six months; the yield is more than 94%; the content is more than 20%; no three wastes and other wastes are produced in the whole production technology, so that the production technology is clean and environmentally friendly.

Description

technical field [0001] The invention relates to a preparation method of a strong basic catalyst and an ethoxylation agent in the medicine and pesticide industry, and more specifically relates to a preparation method of sodium ethylate. Background technique [0002] Sodium ethoxide is a white or light yellow hygroscopic powder, mainly used as a strong basic catalyst, ethoxylation agent, and as a coagulant and reducing agent in organic synthesis and pharmaceutical synthesis. The pharmaceutical products that use sodium ethoxide include phenbital, phenylbutazone, primidone, methyldopa, tetracaine hydrochloride, yikezine, aminopterin, pyrimethamine, and pivuracillin, etc. In addition, it is also used in pesticides and as analytical reagents. At present, the large-scale production methods of sodium ethoxide at home and abroad include benzene dehydration azeotropic method and water absorption dehydration method. [0003] The traditional process uses benzene as an entrainer and de...

Claims

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Application Information

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IPC IPC(8): C07C31/30C07C29/70
CPCC07C29/70C07C31/30
Inventor 李华振于西波张陆军王丽波李保铃
Owner SHANDONG HUIHAI PHARMA & CHEM
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