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Production technology for preparing citronellyl nitrile from citronellal

A production process and citronellal technology are applied in the field of production technology for preparing citronellal from citronellal, which can solve the problems of large energy loss, environmental pollution by waste acid water, strong corrosiveness, high price and the like, and reduce labor intensity. , The effect of improving economy and reducing production cost

Active Publication Date: 2015-04-22
广州百花香料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthesis process has the disadvantages of strong corrosiveness and high price of the raw material hydroxylamine, and the energy consumption is large in the production process, and the waste acid water produced pollutes the environment.

Method used

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  • Production technology for preparing citronellyl nitrile from citronellal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 5-liter reaction kettle, add 785 g of isopropanol and 230 g of citronellal to mix, use nitrogen to remove the air in the kettle three times, control the reaction temperature at 15°C~25°C, quickly add 18 g of cobalt chloride and dropwise 364 g 25% ammonia water. Continue to control the temperature of the reaction solution at 15-25°C, add 340 g of 50% hydrogen peroxide, and track the reaction of citronellal with chromatography after the dropwise addition until the content of citronellal is less than 1.0%. After the reaction was completed, acetic acid was added to neutralize the reaction solution (PH = 7-8), the solvent was recovered, and 226 g of citronellolonitrile was obtained after purification, with a content of 97.6% and a yield of 87.2%.

Embodiment 2

[0022] In a 5-liter reaction kettle, add 785 g of isopropanol and 230 g of citronellal to mix, use nitrogen to remove the air in the kettle three times, control the temperature of the reaction solution at 15~25°C, quickly add 10 g of cuprous chloride and drop 425 g 25% ammonia water. Control the temperature of the reaction solution at 15-25°C, add 192 g of 50% hydrogen peroxide, and react until the citronellal content is less than 1.0% after the dropwise addition. After the reaction was completed, acetic acid was added to neutralize the reaction solution (PH = 7-8), the solvent was recovered, and 219 g of citronellyl nitrile product was obtained after purification, with a content of 98.1% and a yield of 85.0%.

Embodiment 3

[0024] In a 5 liter reactor, mix 785 g of isopropanol and 230 g of citronellal. Use nitrogen to remove the air in the kettle three times, control the temperature of the reaction solution at 3~15°C, quickly add 15 g of copper chloride and 387 g of 25% ammonia water dropwise. Control the temperature of the reaction solution at 3-15°C, add 192 g of 50% hydrogen peroxide dropwise, and react until the citronellal content is less than 1.0%. After the reaction was completed, acetic acid was added to neutralize the reaction solution (PH=7-8), the solvent was recovered, and 218 g of citronellonitrile product was obtained after purification, with a content of 97.8% and a yield of 85%.

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Abstract

The invention relates to a production technology for preparing citronellyl nitrile from citronellal. The technology comprises the following steps: mixing citronellal with isopropanol in a same reaction kettle, controlling the reaction temperature in a range of -5-35DEG C, quickly adding a catalyst and 25% ammonia water, adding an oxidant in a dropwise manner under a controlled speed within 2-4h, neutralizing after the above reaction, carrying out solvent recovery, and purifying to obtain a citronitrile product with the yield of above 83%and the purity of above 97%, wherein the catalyst is chloride, iodide, nitrate or sulfate of copper, cobalt, silver or vanadium, and the oxidant is lead nitrate, manganese dioxide, hydrogen peroxide, ozone, oxygen or chromium trioxide. The technology for preparing citronellyl nitrile from citronellal adopts citronellal as a raw material and isopropanol as a solvent, utilizes a one-pot catalytic ammoxidation reaction technique and optimizes a ratio, so the technology provided by the invention has the advantages of simplified process operation flow, shortened production cycle, reduction of the labor intensity and the production cost, and environmental protection.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and specifically refers to a production process for preparing citronellyl nitrile from citronellal. Background technique [0002] Citronellal has a strong citrus and lemon-like aroma, and has an aldehyde aroma, and the aroma is specific, strong and long-lasting. It is especially suitable for the formulation of soap essence and synthetic detergent essence, and can also be used for the fragrance of other daily chemical products. Moreover, citronella nitrile also has the functions of repelling mosquitoes and repelling insects, and is an important nitrile fragrance with great development value. [0003] At present, the process for preparing citronellyl nitrile from citronellal mainly adopts the hydroxamin oximation method: the reaction of citronellal with hydroxylamine produces citronellal oxime. Then, use acetic anhydride as a dehydrating agent to obtain citronellyl nitrile by dehydration u...

Claims

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Application Information

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IPC IPC(8): C07C255/07C07C253/26
Inventor 张建斌王烨
Owner 广州百花香料股份有限公司
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