CN105985315A - Method for extracting nicotine from tobacco waste - Google Patents

Method for extracting nicotine from tobacco waste Download PDF

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Publication number
CN105985315A
CN105985315A CN201510061903.5A CN201510061903A CN105985315A CN 105985315 A CN105985315 A CN 105985315A CN 201510061903 A CN201510061903 A CN 201510061903A CN 105985315 A CN105985315 A CN 105985315A
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nicotine
tobacco leftovers
filtrate
extractant
extraction
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CN201510061903.5A
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Chinese (zh)
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杨晓林
李鑫伟
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Individual
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Abstract

The invention relates to a method for extracting nicotine from tobacco waste. The method comprises the following steps: pretreatment of the tobacco waste, extraction of a processing material, and purification of nicotine. The method has the characterisitics that the steps are simple, the nicotine extraction rate is high, and the cost is low. The method for extracting nicotine from tobacco waste can be widely used for a high-efficient pesticide and a biopesticide for the crops.

Description

The extracting method of nicotine in a kind of tobacco leftovers
Technical field
The present invention relates to agricultural wastes technical field of resource recovery, the extracting method of nicotine in a kind of tobacco leftovers.
Background technology
From Discarded Tobacco leftover bits and pieces, extract natural nicotine, be the major way of Nicotiana tabacum L. comprehensive utilization.Traditional alkaloid extracting method is built upon the physicochemical property of alkaloid, include the solubility property of acid, alkali etc. especially for different solvents on the basis of.In general, can use steam distillation except minority has volatile alkaloid, the alkaloid with sublimability can use outside sublimed method extraction, and most alkaloids utilize solvent extraction method and ion-exchange-resin process to extract.The typically extraction and two processes of purification by alkaloid of extraction process forms.
Solvent extraction has India, Turkey's productivity patent report the earliest, and China is also carried out the exploration of this respect.Its technical process is to use lime cream treatment and purification after Nicotiana tabacum L. immersion, uses Na2CO3Ca except remaining2+Ion, the organic solvent extractions such as clear liquor chloroalkene (trichloro ethylene, chloroform, dichloropropylene etc.), ether, chloroform, solvent naphtha, extract sulphuric acid eluting, nicotine is transferred to aqueous phase from organic facies and is become nicotine neutral sulfate., is repeatedly enriched with to obtain nicotine neutral sulfate. product.
The feature of ion-exchange-resin process is that direct clear water soaks Nicotiana tabacum L., the acylate aqueous solution of nicotine is obtained after filtration, then this solution is flowed through ion exchange resin (strong-acid type), nicotine is i.e. enriched on ion exchange column, then i.e. obtains the aqueous solution Yin of free nicotine with alkali exchange.The technological process of ion-exchange-resin process is generally: dilute sulfuric acid immersions → filtration → ion exchange → hydrochloric acid solution eluting → add NaOH solution adjustment pH value → kerosene extraction → sulphuric acid back extraction → nicotine neutral sulfate. → be refining to obtain high-purity nicotine.Ion exchange resin is generally storng-acid cation exchange resin, Dowex50w-x $ type resin, HN268 type cation exchange resin etc..This method can obtain the nicotine that comparison is pure;But the production cycle is long, product loss is serious, and resin is easily poisoned, and is unfavorable for commercial introduction.
Such as CN103102340A Chinese invention patent discloses prepares nicotine with dilution heat of sulfuric acid percolation.Use the method can conveniently obtain the nicotine products that purity is 76%, simplify technique, decrease chloroform usage amount, save equipment investment, energy efficient simultaneously, there is important society and economic implications.
Such as CN1234403A Chinese invention patent discloses a kind of nicotine and extracts row technique, Nicotiana tabacum L. is first used hot water extraction, more successively adds C in lixiviating solutiona(OH)2And CO2It is neutralized, filtering after neutralization, filtrate i.e. refining smoke succus ethyl acetate or chloroform extracts in packed tower, and evaporation is to obtain containing free nicotine 75~85%, evaporation raffinate phase, to reclaim extractant, makes raffinate phase can be recycled as extraction hot water.This process equipment is simple, easy to operate, without waste water, discarded, waste material generation, meets industrialization production requirements.
Wang Xianke etc. propose new liquid-film method and separate, extract the method that Buddhist nun accounts for fourth, and this system N, N-DOAA di sec octylacetamide, sec-octyl alcohol (octanol-2) are flowing carrier, LIl3B (diene succimide) is that surfactant, sulfonated kerosene make solvent, H2SO4Aqueous solution makees interior phase reagent, uses different liquid-film methods to extract nicotine sulfate and high pure nicotine, measures through test center of the Chinese Academy of Sciences, purity up to more than 99%.The method is currently in laboratory stage, and yield is little, and cost is high.
Summary of the invention
Patent of the present invention to solve the technical problem that: provides the extracting method of nicotine in a kind of tobacco leftovers.Using alkali liquor restricted-access media nicotine, extracting solution uses non-polar solven repeatedly to extract, and obtains the purity nicotine products more than 92% after purification.
After crushing in view of tobacco leftovers, when Nicotiana tabacum L. size is more than 8mm, nicotine is difficult to from Nicotiana tabacum L. extraction and extraction time is elongated, adds energy resource consumption, so Nicotiana tabacum L. size 8mm after Fen Suiing.
The consumption of extract when extracting in view of nicotine, when the mass ratio of filtrate and extract is less than 1:0.3, not exclusively, partial nicotinic is not extracted completely in extraction;When the mass ratio of filtrate and extract is more than 1:0.5, extractant consumption is relatively big, and causes waste, so the mass ratio of filtrate and extract controls between 1:0.3~0.5.
Low in view of Extracting temperature, directly influence yield low,;Extracting temperature is too high, can directly damage working substance, so Extracting temperature is at 50~70 DEG C.
The extracting method of nicotine in described a kind of tobacco leftovers, it is characterised in that technological process is as follows:
(1) pre-treatment of tobacco leftovers: the tobacco leftovers collected is pulverized and is dried, Nicotiana tabacum L. size 8mm after pulverizing, the NaOH solution that concentration is 4.7~8.5% is added by certain solid-liquid ratio, 3~6h are stirred with rotating speed 200~350rpm in 50~70 DEG C of water-baths, then, it is cooled to room temperature, filters, collect filtrate;
(2) process the extraction of material: join in filtrate according to the mass ratio of 1:0.3~0.5 by extractant, earthquake machine shakes 2min, takes upper layer of extraction liquid, repeat filtrate to extract one time, combining extraction liquid;
(3) purification of nicotine: filtrate is distilled under 70~80 DEG C of environment, remove extractant and obtain nicotine crude product, according to volume ratio 1:3~6, nicotine crude product and extractant are mixed, add appropriate palmitic acid and distilled water, 5h it is incubated under the conditions of 35~45 DEG C, citric acid with 15% regulates PH to 10, decompression distillation, the nicotine products after being refined.
Having the advantages that of this invention: (1), compared with traditional extraction process, the technological process of the present invention is substantially shortened, efficiency improves, and production cost reduces so that investment reduces, and reduce further its production cost;(2) there is not the pollution to environment during extracting, select environmental protection raw material, friendly process, product also supports energy-conservation requirement;(3) Novel tobacco alkaline extraction technology is entirely autonomous innovative technology, and breaks through foreign technology fetters, for improving technological level, eliminating the reliance on foreign technology and contribute;(4) develop novel plant extraction process technology, reach energy-saving and cost-reducing purpose simultaneously.
Detailed description of the invention
Will assist in understand the present invention by following enforcement operation and embodiment, but be not limiting as present disclosure.
Embodiment 1-4
(1) pre-treatment of tobacco leftovers: pulverized by the tobacco leftovers of collection and dry, pulverize rear Nicotiana tabacum L. size 8mm, adding NaOH solution concentration by certain solid-liquid ratio is 4.7~8.5%, stirs 3~6h with rotating speed 200~350rpm in 50~70 DEG C of water-baths;It is then cooled to room temperature, filter, collect filtrate;
(2) process the extraction of material: join in filtrate according to the mass ratio of 1:0.3~0.5 by extractant, earthquake machine shakes 2min, takes upper layer of extraction liquid, repeat filtrate to extract one time, combining extraction liquid;
(3) purification of nicotine: filtrate is distilled under 70~80 DEG C of environment, remove extractant and obtain nicotine crude product, according to volume ratio 1:3~6, nicotine crude product and extractant are mixed, add appropriate palmitic acid and distilled water, 5h it is incubated under the conditions of 35~45 DEG C, citric acid with 15% regulates PH to 10, decompression distillation, the nicotine products after being refined.
Table 1 nicotine extracts inventory
The technique table that table 2 nicotine extracts

Claims (4)

1. the extracting method of nicotine in a tobacco leftovers, it is characterised in that technological process is as follows:
(1) pre-treatment of tobacco leftovers: the tobacco leftovers collected is pulverized and is dried, Nicotiana tabacum L. size 8mm after pulverizing, the NaOH solution that concentration is 4.7~8.5% is added by certain solid-liquid ratio, 3~6h are stirred with rotating speed 200~350rpm in 50~70 DEG C of water-baths, then, it is cooled to room temperature, filters, collect filtrate;
(2) process the extraction of material: join in filtrate according to the mass ratio of 1:0.3~0.5 by extractant, earthquake machine shakes 2min, takes upper layer of extraction liquid, repeat filtrate to extract one time, combining extraction liquid;
(3) purification of nicotine: filtrate is distilled under 70~80 DEG C of environment, remove extractant and obtain nicotine crude product, according to volume ratio 1:3~6, nicotine crude product and extractant are mixed, add appropriate palmitic acid and distilled water, 5h it is incubated under the conditions of 35~45 DEG C, citric acid with 15% regulates PH to 10, decompression distillation, the nicotine products after being refined.
The extracting method of tobacco leftovers the most according to claim 1, it is characterised in that the feed liquid mass ratio of described tobacco leftovers and NaOH solution is 1:7.5~8.5.
The extracting method of tobacco leftovers the most according to claim 1, it is characterised in that described extractant is non-polar solven, such as normal hexane or pentane or normal heptane or the mixture of several non-polar solven.
The extracting method of tobacco leftovers the most according to claim 1, it is characterised in that quality is gross mass the 5.5~7.5% of described addition palmitic acid.
CN201510061903.5A 2015-02-06 2015-02-06 Method for extracting nicotine from tobacco waste Pending CN105985315A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107149161A (en) * 2017-07-20 2017-09-12 安徽中烟工业有限责任公司 A kind of low nicotine tobacco extract and preparation method thereof
CN107311976A (en) * 2017-08-03 2017-11-03 湖北和诺生物工程股份有限公司 A kind of intermediate extraction element and method
CN109512014A (en) * 2017-09-18 2019-03-26 湖南中烟工业有限责任公司 A method of the extraction nicotine from tobacco
CN110903277A (en) * 2018-09-18 2020-03-24 河南元萃生物科技有限公司 Method for saponifying and hydrolyzing tobacco leaves by ultrasonic alkaline water and extracting nicotine by reduced pressure distillation
CN111978290A (en) * 2020-08-24 2020-11-24 云南农业职业技术学院 Method for extracting high-purity nicotine from tobacco waste

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Publication number Priority date Publication date Assignee Title
CN1032165A (en) * 1988-03-09 1989-04-05 洛阳师范专科学校教务处 Extraction nicotine from tobacco
CN1064680A (en) * 1992-03-07 1992-09-23 吴景峰 The production technique of nicotine salt and pure nicotine products
CN104086425A (en) * 2014-07-30 2014-10-08 中国农业科学院烟草研究所 Method for simultaneously extracting and separating chlorogenic acid, solanesol, alkaloid and rutin in tobacco

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN1032165A (en) * 1988-03-09 1989-04-05 洛阳师范专科学校教务处 Extraction nicotine from tobacco
CN1064680A (en) * 1992-03-07 1992-09-23 吴景峰 The production technique of nicotine salt and pure nicotine products
CN104086425A (en) * 2014-07-30 2014-10-08 中国农业科学院烟草研究所 Method for simultaneously extracting and separating chlorogenic acid, solanesol, alkaloid and rutin in tobacco

Non-Patent Citations (1)

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Title
王美兰: "烟碱的提取与纯化", 《万方学位论文数据库》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107149161A (en) * 2017-07-20 2017-09-12 安徽中烟工业有限责任公司 A kind of low nicotine tobacco extract and preparation method thereof
CN107149161B (en) * 2017-07-20 2018-07-10 安徽中烟工业有限责任公司 A kind of low nicotine tobacco extract and preparation method thereof
CN107311976A (en) * 2017-08-03 2017-11-03 湖北和诺生物工程股份有限公司 A kind of intermediate extraction element and method
CN109512014A (en) * 2017-09-18 2019-03-26 湖南中烟工业有限责任公司 A method of the extraction nicotine from tobacco
CN110903277A (en) * 2018-09-18 2020-03-24 河南元萃生物科技有限公司 Method for saponifying and hydrolyzing tobacco leaves by ultrasonic alkaline water and extracting nicotine by reduced pressure distillation
CN111978290A (en) * 2020-08-24 2020-11-24 云南农业职业技术学院 Method for extracting high-purity nicotine from tobacco waste

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