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Preparation method of high purity nicotine

A high-purity, nicotine technology, which is applied in the field of separation and purification of natural biological products, can solve the inevitable problems such as naphthalene impurities, and achieve the effect of high product purity, positive smell, and avoiding impurities

Active Publication Date: 2016-05-11
北京本草通汇科技中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the easy saponification of naphthalene impurities in alkaline water, the nicotine prepared by this method inevitably has naphthalene impurities that have a boiling point similar to that of nicotine and are difficult to remove.

Method used

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  • Preparation method of high purity nicotine
  • Preparation method of high purity nicotine
  • Preparation method of high purity nicotine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The preparation method of the high-purity nicotine of the present embodiment comprises the following steps:

[0040] (1) Take 400L of crude nicotine containing methylnaphthalene with a purity of 97% in a 2000L extraction tank, add an equal volume of No. 6 reagent oil, mix well, add 400L of deionized water, oscillate, stand and separate, and collect the water phase Layer, repeatedly added deionized water to extract 6 times, combined the aqueous layer, the gas chromatography-mass spectrum of its nicotine solution is as follows figure 1 shown. Take 2400L of the aqueous phase layer solution, add 600L of No. 6 reagent oil, oscillate, stand for stratification, collect the No. 6 reagent oil layer, repeatedly add No. 6 reagent oil for extraction 4 times, merge the No. 6 reagent oil layer nicotine solution, and the gas phase of the nicotine solution Chromatography-mass spectrum such as figure 2 shown.

[0041] (2) Take 500L of primary purified nicotine solution, put it in a ...

Embodiment 2

[0046] The preparation method of the high-purity nicotine of the present embodiment comprises the following steps:

[0047] (1) Take 10L of crude nicotine that does not contain oil-soluble impurities such as naphthalene that has a similar boiling point to nicotine, and has a purity of 98%, pour it into a short-range molecular still, and control the vacuum degree of the first-stage vacuum distillation pump at 0.1mbar Around, the temperature is controlled at 60°C, the vacuum degree of the second-stage vacuum distillation pump is controlled at 0.08mbar, and the temperature is controlled at 35°C, and finally nearly colorless and transparent high-purity nicotine is obtained.

[0048] The components and content of the collected high-purity nicotine were analyzed by GC-MS, and the impurities were basically removed, while the content of nicotine could reach 99.86%, the moisture content was only 0.05%, and the yield

[0049] 91.8%.

Embodiment 3

[0051] The preparation method of the high-purity nicotine of the present embodiment comprises the following steps:

[0052] (1) Use 100 L of No. 6 solvent oil to extract 100 kg of waste shredded tobacco leaves for 2 to 4 hours in an extraction tank with temperature control at 50-80° C., and take out the tobacco leaves.

[0053] (2) Place the extracted nicotine solution in a solvent evaporator, adjust the vacuum of the solvent evaporator to about 100mbar, control the temperature at 45°C, cool the circulating water at -10°C, and concentrate the solvent. In order to avoid the deterioration of nicotine exposed to light, the entire solvent evaporator is shielded with a black plastic film.

[0054] (3) Pour the concentrated solution into a short-range molecular still, control the vacuum degree of the first-stage vacuum distillation pump at about 0.1mbar, and control the temperature at 50°C, turn off the second-stage vacuum distillation pump, first distill out the solvent part, and t...

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Abstract

The invention relates to natural biological product separation and purification and concretely relates to a preparation method of high purity nicotine. The preparation method comprises pouring a nicotine organic solution without naphthalene oil-soluble impurities and high-boiling point alkaloid impurities into a short-path molecular distillation device and carrying out rectification on the nicotine organic solution at a temperature of 0-100 DEG C under pressure of 0.001-1mbar to obtain high purity nicotine. The invention provides a method for removing naphthalene oil-soluble impurities with boiling points similar to that of nicotine and high-boiling point alkaloid impurities in nicotine through extraction-back extraction. The preparation method is carried out at a low temperature at a high degree of vacuum and prevents impurities produced through nicotine pyrolysis and oxidation. The product has purity of 99.92%, good appearance, a good smell and a high extraction yield.

Description

technical field [0001] The invention relates to the separation and purification of natural biological products, in particular to a method for preparing high-purity nicotine. Background technique [0002] Nicotine, also known as nicotine, is an important pharmaceutical and chemical raw material. It is expected to become an effective drug for the treatment of Alzheimer's disease, Parkinson's disease, and depression. Above 1 million yuan / ton. At present, nicotine is mainly extracted from tobacco or waste tobacco stems and tobacco leaves. [0003] Nicotine is easily soluble in alcohol, ether, chloroform, alkanes and other organic solvents and water. In industry, it is mainly used for extraction in solvent oil with a rotary furnace, or in an extraction tank for extraction in lye or acid solution. After removing the solvent, pass Rectification obtains higher purity nicotine. Since the rectification temperature of the industrial rectification tower is generally above 100°C, the ...

Claims

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Application Information

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IPC IPC(8): C07D401/04
Inventor 刘金龙郑威陈家任毕文钢王安江
Owner 北京本草通汇科技中心
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