Method for preparing policosanol mixture by nonsolvent reduction method

A technology for preparing higher alkanols and higher alkanols is applied in the preparation of organic compounds, chemical instruments and methods, preparation of oxygen-containing compounds, etc., and can solve the problems of difficult control of reaction conditions, unfavorable safe production, increased production costs, etc. The effect of easy control of process conditions, low cost and high safety

Inactive Publication Date: 2009-03-18
THE RES INST OF RESOURCES INSECTS RIRI OF THE CHINESE ACADEMY OF FORESTRY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has disadvantages such as relatively complex process, large use of organic solvents, uneasy control of reaction conditions, and low conversion rate, whic

Method used

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  • Method for preparing policosanol mixture by nonsolvent reduction method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A. Weigh 10 g of commercially available white wax, put it in a 200 ml beaker, heat it on an electric furnace to 84 ° C, then add 1.0 g of lithium aluminum hydride under continuous stirring, and keep the temperature for 10 minutes to obtain a mixture;

[0032] B. Slowly add 100g of tap water to the mixture in step A, continue stirring, heat to boiling, slowly add 1g of 0.5mol / L HCl solution, and heat to boiling for 10min;

[0033] C. When cooling to 50°C, the solid and liquid phases are separated, and the upper layer is taken out to obtain the crude product of the higher alkanol mixture;

[0034] D. Put the crude higher alkanol mixture taken out into 150g tap water, add 0.1g0.5mol / L HCl solution, heat and boil for 10min, then adjust the pH value to neutral with 0.1mol / L NaOH solution, and cool to room temperature , so that the solid and liquid phases are separated, the solid phase is the higher alkanol mixture product, and 9.5 g of the higher alkanol mixture product is o...

Embodiment 2

[0036] A. Weigh 20g of commercially available paraffin wax and put it into a 500ml beaker, heat it on an electric furnace to 100°C, then add 1.0g Ranny-Ni under the condition of continuous stirring, and keep the temperature for 60min to obtain the mixture;

[0037] B. Slowly add 400g of tap water to the mixture in step A, continue stirring, heat to boiling, add 10g of 0.5mol / L HCl solution, and heat to boiling for 20min;

[0038] C. When cooled to 55°C, the solid and liquid phases are separated, and the upper layer is taken out to be the crude product of higher alkanol mixture;

[0039]D. Put the crude product of the higher alkanol mixture taken out into 400g tap water, add 1.0g0.5mol / L HCl solution, heat and boil for 20min, adjust the pH value to neutral with 0.2mol / L NaOH solution, cool to normal temperature, and make solid , liquid phase separation, the solid phase is the higher alkanol mixture product, and the higher alkanol mixture product is weighed to obtain 19.3g, with...

Embodiment 3

[0041] A. Weigh 50g of commercially available white wax and put it in a 2000ml stainless steel pot, heat it on an electric stove to 120°C, add 1.6g of lithium aluminum hydride under continuous stirring, and keep the temperature for 100min to obtain a mixture;

[0042] B. Slowly add 1500g of tap water to the mixture in step A, continue stirring, heat to boiling, slowly add 50g of 0.5mol / L HCl solution, and heat to boiling for 30min;

[0043] C. When cooling to 60°C, the solid and liquid phases are separated, and the crude product of the higher alkanol mixture in the upper layer is taken out;

[0044] D, put the crude product of the higher alkanol mixture taken out into 1500g tap water, add 5g0.5mol / L HCl solution, heat and boil for 30min, adjust the pH value to neutrality with 0.5mol / L NaOH solution, cool to normal temperature, make solid , liquid phase separation, the solid phase is the product of the higher alkanol mixture, and 47.0 g of the higher alkanol mixture was obtaine...

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Abstract

The invention provides a method for preparing advanced alkanol mixtures through a non-solvent reduction method. The method is characterized in that Chinese wax which is biological wax is taken as a raw material; a reducing agent is added to the Chinese wax according to that the mass ratio of the reducing agent to the Chinese wax is between 1 to 10 and 30 under the condition of adding no organic solvent and in an atmospheric-pressure open system; water is added according to that the mass ratio of the Chinese wax to the water is between 1 to 10 and 30; the materials are stirred and heated to boil; 0.5mol/L HCl solution is added according to that the mass ratio of the Chinese wax to the HCl solution is between 1 to 0.1 and 1, is heated to boil for 10 to 30 minutes, and then is cooled to between 50 and 60 DEG C for separating solid-liquid phase; matter in an upper layer is an advanced alkanol mixture; water and hydrochloric acid solution are added and boiled for 10 to 30 minutes; the pH value of the mixture is adjusted to be neutral; and the mixture is cooled to normal temperature, and then an advanced alkanol mixture product is obtained. The method has the advantages of simple process, easy operation, environment-friendly property, safety, low cost and high reaction conversion rate.

Description

technical field [0001] The invention relates to a method for preparing a higher alkanol mixture, in particular to a method for preparing a higher alkanol mixture by a non-solvent reduction method using pyrethrum as a raw material. Background technique [0002] Higher alkanols, also known as higher fatty alcohols, are chain-like saturated monohydric alcohols containing more than twelve carbon atoms. It exists widely in nature, but it hardly exists in the form of natural free fatty alcohols, but in the form of wax esters. Wax esters rich in higher alkanols include: rice bran wax, sugarcane wax, sorghum wax, insect wax, beeswax, carnauba wax, sunflower wax, shellac wax, wool wax, etc. Research on higher alkanols at home and abroad focuses on C 22 ~C 36 Preparation, separation and utilization of mixed alcohols and other technical fields. Docosanol in the higher alkanol mixture can be used to inhibit prostate tumors; tetracosanol can enhance the function of nerve factors; , ...

Claims

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Application Information

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IPC IPC(8): C07C27/02C07C31/02
Inventor 陈晓鸣段琼芬张重权马李一王有琼
Owner THE RES INST OF RESOURCES INSECTS RIRI OF THE CHINESE ACADEMY OF FORESTRY
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