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A kind of preparation method of high-purity nicotine

A nicotine and temperature control technology, applied in the field of separation and purification of natural biological products, can solve problems such as unavoidable naphthalene impurities, and achieve the effects of high product purity, avoidance of impurities and positive odor.

Active Publication Date: 2018-10-16
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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  • A kind of preparation method of high-purity nicotine
  • A kind of preparation method of high-purity nicotine
  • A kind of preparation method of high-purity nicotine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The preparation method of high-purity nicotine in this embodiment includes the following steps:

[0040] (1) Take 400L of crude nicotine containing methyl naphthalene 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, shake, stand for layering, and collect the water phase Layer, repeatedly add deionized water for extraction 6 times, combine the water layer, the gas chromatography-mass spectrogram of the nicotine solution is as follows figure 1 Shown. Take 2400L of the aqueous layer solution, add 600L of No. 6 reagent oil, shake, stand for layering, collect No. 6 reagent oil layer, repeatedly add No. 6 reagent oil to extract 4 times, combine the No. 6 reagent oil layer nicotine solution, the nicotine solution Gas chromatography-mass spectrogram such as figure 2 Shown.

[0041] (2) Take 500L of the primary purified nicotine solution and place it in a solvent evaporator, adjust the vacuum degree of...

Embodiment 2

[0046] The preparation method of high-purity nicotine in this embodiment includes the following steps:

[0047] (1) Take 10L of crude nicotine with a purity of 98% without oil-soluble impurities such as naphthalene, which is similar to the boiling point of nicotine, and pour it into a short-path molecular distiller, and control the vacuum degree of the first-class vacuum distillation pump to 0.1mbar The temperature is controlled at 60°C, the vacuum degree of the second-class vacuum distillation pump is controlled at 0.08mbar, and the temperature is controlled at 35°C. Finally, a colorless and transparent high-purity nicotine is obtained.

[0048] The components and content of the collected high-purity nicotine are analyzed with a gas-mass spectrometer. The impurities are basically removed, and the nicotine content can reach 99.86%, the moisture content is only 0.05%, and the yield is

[0049] 91.8%.

Embodiment 3

[0051] The preparation method of high-purity nicotine in this embodiment includes the following steps:

[0052] (1) Use 100L of solvent oil No. 6 in the extraction tank to control the temperature at 50~80℃ to extract 100kg of waste and broken tobacco leaves for 2~4h, and then take out the tobacco leaves.

[0053] (2) Put the extracted nicotine solution in a solvent evaporator, adjust the vacuum degree of the solvent evaporator to about 100mbar, control the temperature at 45°C, cool the circulating water temperature at -10°C, and concentrate the solvent. In order to prevent nicotine from being degraded by light, the entire solvent evaporator is shaded with black plastic film.

[0054] (3) Pour the concentrated liquid into the short-path molecular distiller, control the vacuum degree of the first-class vacuum distillation pump at about 0.1mbar and the temperature at 50℃, turn off the second-class vacuum distillation pump, first distill the solvent part, and then turn it on The second-...

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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. Its demand is large. Nicotine with a purity of 99.9% is sold at home and abroad. Above 1 million yuan / ton. At present, nicotine is mainly extracted from tobacco or tobacco stems and tobacco leaves discarded from tobacco production. [0003] Nicotine is easily soluble in organic solvents such as alcohol, ether, chloroform, alkanes, and water. In industry, it is mainly used for extraction in mineral spirits with a flat converter, or extraction in lye or acid with an extraction tank, and passes through after removing the solvent. Rectification to obtain higher purity nicoti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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