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Method for preparing 10 - hydroxy capric acid

A technology for the synthesis of hydroxydecanoic acid, which is applied in chemical instruments and methods, preparation of carboxylate salts, and preparation of organic compounds. Safe production, high heating efficiency, and energy-saving effects

Inactive Publication Date: 2007-12-26
GUANGDONG IND TECHN COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Li Kai et al. used 95% ethanol under high pressure to crack the yield of 70%; Huang Xiaofeng et al. used 2-octanol and water to acidify the yield to 75% for 6 hours. The first reaction process was cumbersome and the yield was low, and the latter three Although the reaction yield is high, there are characteristics such as high requirements for equipment withstand voltage, long reaction time, and complicated process.
[0004] The technical conditions for the industrial production of the existing 10-hydroxydecanoic acid are: temperature 200±5°C, pressure 3~4Mpa, and initial reaction time 12 hours. Therefore, there are also the disadvantages of high reaction temperature, high pressure and long time. Poor production safety, large power consumption and low production efficiency

Method used

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  • Method for preparing 10 - hydroxy capric acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 14g castor oil is mixed with 6g secondary octanol, and the mixture of above-mentioned castor oil and secondary octanol is dripped into microwave (microwave frequency is 2450MHz; microwave power is 300W) radiated to 15g secondary octanol under 120 ℃ at a constant rate of 1mL / min. In a mixture of octanol and 20 g of 75% (mass percentage) sodium hydroxide, stir evenly, keep the same microwave frequency and power, continue microwave radiation to make the reaction temperature 150-180° C., and keep reflux for 1 h. After the reaction, add 60mL of water to wash away the alkali and remove the water layer; the oil layer was extracted 4 times with hot water at 80-85°C, and the water layers were combined and acidified to pH 6.0-6.5 with 60-70% (mass percent) sulfuric acid, cooled To 30 ~ 40 ℃, continue to acidify until the Congo red test paper turns blue. Stand still for 4 hours, filter with suction, and dry at 65°C to obtain solid 10-hydroxydecanoic acid, the yield is: 4.5g, and t...

Embodiment 2

[0020] Castor oil 14g is mixed with 14g secondary octanol, and the mixture of above-mentioned castor oil and secondary octanol is dripped into microwave (microwave frequency is 2450MHz; Microwave power is 200W) radiation to 21g secondary octanol under 110 ℃ with 3mL / min drop rate In a mixture of 25 g of octanol and 70% (mass percentage) sodium hydroxide, stir evenly, continue microwave (microwave frequency: 2450 MHz; microwave power: 400 W) radiation to make the reaction temperature: 160-190 ° C, keep reflux for 1.5 h. After the reaction, add 50mL water to wash away the alkali, separate the water layer; extract the oil layer with hot water at 75-85°C for 4 times, and acidify the combined water layer with 60-70% (mass percent) sulfuric acid to pH6.0-6.5, and cool to 30 ~40°C, continue to acidify until the Congo red test paper turns blue. Stand still for 4 hours, filter with suction, and dry at 65°C to obtain solid 10-hydroxydecanoic acid, yield: 5.1 g, yield: 75%. White crysta...

Embodiment 3

[0022] Castor oil 14g is mixed with 4.2g secondary octanol, and the mixture of above-mentioned castor oil and secondary octanol is dripped into microwave (microwave frequency is 2450MHz; Microwave power is 400W) radiation to 21g In the mixture of 2-octanol and 70% (mass percentage) sodium hydroxide 20g, stir evenly, keep the same microwave frequency and power, continue microwave radiation to make the reaction temperature: 150-190°C, keep reflux for 2.5h. After the reaction, add 40mL water to wash away the alkali, separate the water layer; extract the oil layer with hot water at 75-85°C for 4 times, and acidify the combined water layer with 60-70% (mass percent) sulfuric acid to pH6.0-6.5, and cool to 30 ~40°C, continue to acidify until the Congo red test paper turns blue. Stand still for 4 hours, suction filter, and dry at 65°C to obtain solid 10-hydroxydecanoic acid, the yield is: 4.6g, and the yield is: 68%. White crystals are obtained after recrystallization from benzene, ...

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Abstract

This invention discloses a method for synthesizing 10-hydroxyl capric acid. The method comprises: dropping a mixture of castor oil and 2-octanol into a mixed system of 2-octanol and alkali already subjected to microwave radiation, reacting at a high temperature, washing the product with water, extracting with water, acidifying, filtering, and separating to obtain 10-hydroxyl capric acid. The method utilizes microwave to synthesize 10-hydroxyl capric acid, and can selectively heat the target compound, thus has such advantages as high heating efficiency, low energy consumption, short reaction time, normal pressure reaction and high safety.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing 10-hydroxydecanoic acid by using microwaves. Background technique [0002] 10-Hydroxydecanoic acid is an important fine chemical intermediate with a large market demand. It can be used as a raw material to prepare a variety of high value-added products, which are widely used in the fields of medicine, food, health care products, spices, cosmetics, etc. . It is an important intermediate for the synthesis of high-efficiency active substances - 10-hydroxy-2-decenoic acid, 6-(10-hydroxydecanoic acid)-2,3, dimethoxy-5-methylbenzoquinone, and macrocyclic musk body, and can be directly added to cosmetics as a sebum secretion inhibitor. [0003] 10-Hydroxydecanoic acid can be obtained by high-temperature alkaline cracking of ricinoleic acid glyceride. Mikhaibor, M. et al. used secondary acidification to separate the cracked product, and the yield wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/01C07C51/367C07C51/00
Inventor 高虹张国铭黎彧
Owner GUANGDONG IND TECHN COLLEGE
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