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Process for finely purifying high-purity solanesol form coarse cream of solanesol

A solanesol and high-purity technology, which is applied in the field of refining high-purity solanesol by using crude solanesol paste, can solve the problems of low comprehensive utilization, unfavorable solvent reuse, difficulty in industrialized production, etc., and achieves convenient recovery and The effect of reuse, improving the degree of comprehensive utilization, and easy industrial production

Active Publication Date: 2008-10-15
YUNNAN REASCEND TOBACCO TECH GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process still has the following disadvantages: the process is cumbersome, the scale of production is limited, and industrial production is difficult
This patent uses composite solvents for saponification and recrystallization, which is not conducive to the reuse of solvents, and the process is cumbersome
[0010] Most of the above methods need to go through extraction, column chromatography, decolorization and other procedures, the process is relatively complicated, and a variety of solvents are required, and the amount of solvent is large
At the same time, there are also disadvantages such as low yield, high production cost, and low degree of comprehensive utilization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 100 grams of solanesol crude paste (10.15%) obtained by extracting 6# solvent oil, put it in a 2000ML round-bottomed flask, heat and vacuum concentrate to remove 6# solvent oil, add 500 milliliters of ethanol, and then add 1 gram of hydroxide Potassium, stirred and reacted at 50°C for 2 hours, cooled the reacted liquid to 20°C, controlled the temperature to freeze at -5°C for 2 hours, filtered with suction, and the filtrate 1 was used to prepare tobacco absolute. After recovering ethanol from the filter cake, 42.07 g of solanesol crude paste was obtained. Add 6 times the volume of acetone to dissolve, cool to 20°C, filter to remove impurities, recover the filtrate, and cool to 3-5°C, filter to remove impurities, and collect the filtrate at - Stir in an ice-water bath at 2°C to -5°C for 2 hours, and filter to obtain 9.58 g of light yellow solanesol powder crystals with a content of 91.2% and a yield of more than 86%. The remaining mother liquor after crystallization...

Embodiment 2

[0030] Take 100 grams of solanesol crude paste (8.25%) obtained by extracting 6# solvent oil, put it in a 2000ML round bottom flask, heat and vacuum concentrate to remove 6# solvent oil, add 1000 milliliters of ethanol, and then add 5 grams of hydroxide Potassium, stir and react at 70°C for 3 hours, cool the reacted liquid to 15°C, control the temperature and freeze at -13°C for 5 hours, filter with suction, and filtrate 1 is used to prepare tobacco absolute; filter cake to recover ethanol After that, 41.2 grams of solanesol crude paste was obtained. Add 10 times the volume of acetone to dissolve, cool to 15°C, filter to remove impurities, recover the filtrate, and cool to 3-5°C, filter to remove impurities, collect the filtrate at -2°C to - After stirring in an ice-water bath at 5°C for 5 hours, light yellow crystals were precipitated, and 7.95 g of light yellow solanesol powdery crystals were obtained by filtration, with a content of 90.3%. The yield is greater than 87%. Th...

Embodiment 3

[0032] Get 150 grams of solanesol thick paste (9.01%) obtained by petroleum ether extraction, place in a 2000ML round-bottomed flask, heat and vacuum concentrate to remove petroleum ether, add 1200 milliliters of ethanol, then add 4.5 grams of potassium hydroxide, at 60 Stir and react at ℃ for 3 hours, cool the reacted liquid to 10℃, control the temperature and freeze at -20℃ for 16 hours, filter with suction, and filtrate 1 is used to prepare tobacco absolute; after recovering ethanol from the filter cake, 61.5 Add 8 times the volume of acetone to dissolve the crude cosolaneol paste, cool to 10°C, filter to remove impurities, recover the filtrate, and cool to 3-5°C, filter to remove impurities, collect the filtrate and store it on ice at -2°C to -5°C After stirring in a water bath for 8 hours, light yellow crystals were precipitated, and 12.98 g of light yellow solanesol powdery crystals were obtained by filtration, with a content of 90.6%. The yield is greater than 87%. The...

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PUM

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Abstract

The invention discloses a method for refining the high-purity solanesol by utilizing the solanesol thick paste. The solanesol thick paste is added with ethyl alcohol and potassium hydroxide after low polar solvent is removed from the solanesol thick paste; freezing and filtration are performed after the reaction; after the ethyl alcohol is recycled with a filter cake, the solanesol thick paste is added with acetone for dissolution; cooling, filtering and impurity removal, recooling, filtering and impurity removal are performed to the obtained filtrate; and finally the crystalline mass obtained through freezing and filtering is the required high-purity solanesol. The method has the advantages of simple process, quick separation speed, short production cycle and low solvent loss, and the industrialized production is easy to be realize. The used solanesol has low crude product content, and the mixed solvent is not used during the processes of saponification, impurity removal and edulcoration, thereby greatly facilitating the recycling and the reutilization of the solvent. The tobacco absolute oil can be obtained from the saponated liquid generated during the process of extracting the solanesol through the further separation. Therefore, the comprehensive utilization degree of the wastes is improved.

Description

technical field [0001] The invention belongs to the technical field of intermediate purification, and in particular relates to a method for refining high-purity solanesol by utilizing solanesol crude paste. Background technique [0002] Solanesol (SOLANESOL) is a kind of polyisoprenyl alcohol, the molecular structure is H(CH 2 C(CH 3 )CHCH 2 ) 9 OH, the relative molecular weight is 631, the pure product is a white powdery solid, the melting point is 41 degrees. Solanesol is a long-chain fatty alcohol with weak polarity, easily soluble in organic solvents, but insoluble in water. It mainly exists in the tobacco leaves of flue-cured tobacco, and also contains a small amount of solanesol in potato leaves and mulberry leaves. In production, low-polarity organic solvents are generally used to extract from raw materials containing solanesol to obtain solid or semi-fluid oily solanesol crude paste, which is then subjected to saponification treatment, extraction, decolorization...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/02C07C29/74
Inventor 唐自文刘维涓卫青周瑾
Owner YUNNAN REASCEND TOBACCO TECH GRP
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