Method for purifying nicotine by using subcritical extraction-molecular distillation coupling technique

A technology of molecular distillation and combined technology, which is applied in the direction of organic chemistry, can solve problems such as complex process, and achieve the effect of simple process, less process and low energy consumption

Active Publication Date: 2017-05-31
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method adopts secondary distillation to purify nicotine, and the process is relatively complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The method for purifying nicotine by subcritical extraction-molecular distillation combined technology comprises the following steps:

[0027] 1) Pretreatment: Weigh 1 kg of flue-cured tobacco raw material, place the raw material in a SY-III-A type experimental tobacco processor, spray 20% aqueous sodium carbonate solution (5% by mass fraction) of raw material quality, seal and place for 12h, and make Tobacco leaves are fully absorbed;

[0028] 2) Crush the pretreated material to 10 meshes, use a household microwave oven, microwave at a power of 600W for 30s, and roll it through a rolling-type wall-breaking machine for 3 times to obtain powder;

[0029] Subcritical extraction: add butane (mass ratio 1:8) to the powder, extract at a temperature of 25°C and saturated vapor pressure for 2 hours to obtain an extract;

[0030] The extract is placed in a separation tank, and the solvent is removed by vacuum evaporation to obtain crude nicotine;

[0031] Add 5 times the mass...

Embodiment 2

[0034] The method for purifying nicotine by subcritical extraction-molecular distillation combined technology comprises the following steps:

[0035] 1) Pretreatment: Weigh 1 kg of flue-cured tobacco raw material, place the raw material in a SY-III-A type experimental tobacco processor, spray 5% of the raw material mass in sodium hydroxide aqueous solution (mass fraction 10%), seal it and place it for 6 hours, Make the tobacco leaves fully absorbed;

[0036] 2) Crush the pretreated material to 100 mesh, microwave treatment for 40s at a power of 1200W, and process it for 3 times in total, and then crush it 3 times with a rolling-type wall-breaking machine to obtain powder;

[0037] Subcritical extraction: add dimethyl ether (mass ratio 1:12) to the powder, extract at a temperature of 45°C and saturated vapor pressure for 0.5h to obtain an extract;

[0038] The extract is placed in a separation tank, and the solvent is removed by vacuum evaporation to obtain crude nicotine;

...

Embodiment 3

[0042] The method for purifying nicotine by subcritical extraction-molecular distillation combined technology comprises the following steps:

[0043] 1) Pretreatment: Weigh 1 kg of flue-cured tobacco raw material, place the raw material in a SY-III-A type experimental tobacco processor, spray potassium phosphate aqueous solution (mass fraction 8%) with 15% raw material quality, seal and place for 10h, make Tobacco leaves are fully absorbed;

[0044] 2) Crush the pretreated material to 50 meshes, microwave it for 10s at a power of 800W, and process it for 4 times in total, and grind it 3 times with a rolling-type wall breaker to obtain powder;

[0045]Subcritical extraction: add butane (mass ratio 1:10) to the powder, extract at a temperature of 45°C and saturated vapor pressure for 1.5 hours to obtain an extract;

[0046] The extract is placed in a separation tank, and the solvent is removed by vacuum evaporation to obtain crude nicotine;

[0047] Add 8 times the mass of abs...

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PUM

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Abstract

The invention discloses a method for purifying nicotine by using a subcritical extraction-molecular distillation coupling technique, belonging to the technical field of extraction separation of natural plants. The method mainly comprises three steps of operation: pretreatment of raw materials, subcritical extraction and molecular distillation; in the pretreatment phase of raw materials, an alkaline water solution is sprayed in tobacco leaves, so the existence form of nicotine is changed from a combination form to a free form; nicotine dissolution is accelerated by solvent-less microwave treatment; and combined with the subcritical extraction-molecular distillation coupling technique, the extraction rate and purity of nicotine can be obviously improved. Butane and dimethyl ether are used as extraction agents in subcritical extraction, so the hazard brought about by organic solvents such as ethyl acetate and petroleum ether to operators and environment can be avoided, the safety is good, and the butane and dimethyl ether can be recycled for saving cost. Molecular distillation adopts a low-temperature one-grade distillation technique, and has few processes and small energy consumption. The nicotine purifying process disclosed by the invention is simple, convenient in operation and suitable for large-scale production and application.

Description

technical field [0001] The invention relates to a method for purifying nicotine by using subcritical extraction-molecular distillation combined technology, and belongs to the technical field of natural plant extraction and separation. Background technique [0002] Nicotine is a unique alkaloid in tobacco, and its content accounts for about 95% of the total amount of tobacco alkaloids. It is one of the main indicators for evaluating the quality of tobacco leaves and the main indicator for measuring the taste of cigarettes. High-purity nicotine has good development prospects in the pharmaceutical industry and agricultural fields. For example, in the pharmaceutical field, it is used as a raw material for the development of drugs for the treatment of cardiovascular diseases, skin diseases, snake bites and other diseases. In agriculture, it is mainly used to produce insecticides. agent. [0003] Traditional nicotine extraction methods include steam distillation, organic solvent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 徐秀娟刘珊屈展张文娟霍现宽杨伟平何保江姬凌波胡军宗永立
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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