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Recycling method of waste ethanol obtained through recrystallization of oxadiazon

A technology of recycling and recrystallization, which is applied in chemical instruments and methods, preparation of organic compounds, separation/purification of hydroxyl compounds, etc., can solve the problems of many reaction steps, pollute the environment, increase production costs, etc., and reduce production costs. , Solve the problem, the method is effective and reasonable

Active Publication Date: 2011-07-20
ANHUI KELIHUA CHEM
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Problems solved by technology

[0003] However, the production of oxadiazone technical product has many reaction steps and long process flow, so it is difficult to obtain high-quality products. In order to avoid possible phytotoxicity caused by the small amount of impurities contained in oxadiazone technical product, the product must be refined.
Considering factors such as safety and cost, oxadiazone technical manufacturers generally choose ethanol as the recrystallization solvent, but the recycled ethanol will gradually reduce the concentration of ethanol in the recycled solvent as the number of recycling increases. However, the impurity content gradually increases. The impurity accumulated in the solvent is mainly an organic substance with a unique fragrance of esters, which can form a ternary azeotrope with ethanol and water, and cannot be directly separated, making oxadiazone The refined yield and product purity are greatly reduced. After a certain number of cycles, the recovered ethanol can only be discharged as waste liquid, which not only pollutes the environment but also increases production costs.

Method used

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  • Recycling method of waste ethanol obtained through recrystallization of oxadiazon
  • Recycling method of waste ethanol obtained through recrystallization of oxadiazon
  • Recycling method of waste ethanol obtained through recrystallization of oxadiazon

Examples

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Effect test

Embodiment 1

[0022] see figure 1 300g of waste ethanol (64.5% ethanol, 18.5% organic impurities, 12.6% water, 2.4% chloroform, 2.0% other impurities) produced by recrystallization of oxadiazone was added to a 1000mL three-necked flask with electric stirring, and then 300g newly prepared saturated salt solution, after stirring for 30 minutes, pour the mixed solution into a 1000mL pear-shaped separatory funnel and let it stand for 30 minutes before layering, separating the upper layer of oil (impurity) weighing 49.6g. The lower aqueous solution was transferred to a 1000mL three-neck flask equipped with a thermometer, an electric stirring device and a condenser, and 15.0g of solid sodium hydroxide (96%) was added, stirred for 0.5 to 1 hour, then heated to reflux, refluxed for 2 hours, and used after cooling. Hydrochloric acid neutralized to PH=7. The above hydrolyzate is rectified at atmospheric pressure with a glass rectification device, the main fraction between 77-79°C is collected, and t...

Embodiment 2

[0024] see figure 1 300g of waste ethanol (64.5% ethanol, 18.5% organic impurities, 12.6% water, 2.4% chloroform, 2.0% other impurities) produced by recrystallization of oxadiazone was added to a 1000mL three-necked flask with electric stirring, and then 900g of newly prepared saturated saline solution was stirred for 30 minutes, then the mixed solution was poured into a 2000mL pear-shaped separating funnel and allowed to stand for 30 minutes, and then the layers were separated, and the upper layer of oil (impurity) weighed 38.8g. The lower aqueous solution was transferred to a 1000mL three-neck flask equipped with a thermometer, an electric stirring device and a condenser, and 150.0g of solid sodium hydroxide (96%) was added, stirred for 0.5 to 1 hour, then heated to reflux, refluxed for 4 hours, and used after cooling. Hydrochloric acid neutralized to PH=7. The above hydrolyzate is rectified at atmospheric pressure with a glass rectification device, the main fraction betwee...

Embodiment 3

[0026] see figure 1 300g of waste ethanol (64.5% ethanol, 18.5% organic impurities, 12.6% water, 2.4% chloroform, 2.0% other impurities) produced by recrystallization of oxadiazone was added to a 1000mL three-necked flask with electric stirring, and then 90g of newly prepared saturated aqueous common salt solution was stirred for 30 minutes, and the mixed solution was poured into a 1000mL pear-shaped separatory funnel and allowed to stand for 30 minutes, and then the layers were separated, and the upper layer of oil (impurity) weighed 98.2g. The aqueous solution of the lower layer was transferred to a 1000mL three-neck flask equipped with a thermometer, an electric stirring device and a condenser, and 3.0g of solid sodium hydroxide (96%) was added, stirred for 0.5 to 1 hour, then heated to reflux, refluxed for 2 hours, and used after cooling. Hydrochloric acid neutralized to PH=7. The above hydrolyzate is rectified at atmospheric pressure with a glass rectification device, th...

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Abstract

The invention relates to a recycling method of waste ethanol obtained through the recrystallization of oxadiazon. The recycling method is characterized in that the waste ethanol comprises the following components by weight percent: 40-80% of ethanol, 3-30% of organic matter with special ester aroma, 5-30% of water, 1-10% of chloroform and 1-10% of other impurities; and 95% industrial grade ethanol is prepared through three steps, namely salting-out separation, alkaline hydrolysis and atmospheric distillation. By adopting the method, the waste ethanol obtained through recrystallization of oxadiazon can be recycled to obtain 95% industrial grade ethanol, thus the recovery rate of ethanol can be increased and the production cost can be reduced.

Description

technical field [0001] The invention belongs to a recovery and treatment method of waste solvent, in particular to a recovery and treatment method of waste ethanol produced by recrystallization of oxadiazone. Background technique [0002] Oxadiazone is a selective water-dry dual-purpose herbicide at bud stage, which can control a variety of annual monocotyledonous and dicotyledonous weeds (such as barnyardgrass, bermudagrass, knotweed, etc.), annual Cyperaceae miscellaneous Grass and goosegrass, used in dry land, peanuts, cotton, sugar cane to control barnyard grass, foxtail, etc., has a wide spectrum of weed control, long-lasting and stable drug effects, is not afraid of photolysis, is safe for humans and animals, has good ecological benefits, high efficiency, low toxicity, and low toxicity. Residue, no impact on subsequent crops, welcomed by the majority of users, is one of the herbicide varieties with excellent performance. [0003] However, the production of oxadiazone ...

Claims

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Application Information

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IPC IPC(8): C07C31/08C07C29/76C07C29/80C07C29/88
Inventor 王多余韩谋国王春叶碧陈俊高巍
Owner ANHUI KELIHUA CHEM
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