CN109134180A - A kind of waste tobacco leaf recoverying and utilizing method - Google Patents
A kind of waste tobacco leaf recoverying and utilizing method Download PDFInfo
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- CN109134180A CN109134180A CN201811084248.5A CN201811084248A CN109134180A CN 109134180 A CN109134180 A CN 109134180A CN 201811084248 A CN201811084248 A CN 201811084248A CN 109134180 A CN109134180 A CN 109134180A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07C7/005—Processes comprising at least two steps in series
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- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- C07—ORGANIC CHEMISTRY
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- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
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- C07D401/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
- C07D401/02—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
- C07D401/04—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings directly linked by a ring-member-to-ring-member bond
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Abstract
The invention discloses a kind of waste tobacco leaf recoverying and utilizing method, include the following steps: that just cream must be concentrated in waste tobacco leaf circumfluence distillation by (1)；(2) concentrate is extracted, obtains extract liquor I and raffinate I；The concentration of extract liquor I distillation, saponification, chromatography, decrease temperature crystalline are obtained into Salanesol；(3) loading efflux when collection Salanesol chromatography, obtains neophytadiene after concentration, extraction, distillation；(4) chlorogenic acid medicinal extract is distilled into obtain in the extraction concentration of raffinate I, remaining as raffinate II, chromatographs chlorogenic acid medicinal extract to obtain chlorogenic acid；(5) extraction of raffinate II, concentration distillation, back extraction are obtained into nicotine fine work；(6) it is fermented the addition microorganism of waste residue obtained in step (1) to obtain organic fertilizer.The present invention extracts and separates simultaneously nicotine, chlorogenic acid, Salanesol and neophytadiene, bacterial manure from waste tobacco leaf, and scale production process route fully utilizes the effective component in waste tobacco leaf, and product category is abundant, and economic value is high.
Description
Technical field
The present invention relates to tobacco product processing technique field, in particular to a kind of waste tobacco leaf recoverying and utilizing method.
Background technique
China is tobacco leaf production and the maximum country of consumption figure in the world, accounts for the one third of global total amount or more.Smoking
Harmful to health to have become final conclusion, with the rise of world's tobacco control campaign, purposes of the tobacco in terms of cigarette also will greatly weaken.
However, the natural plant resource as a kind of high yield, the wholesome potential use of tobacco is also very extensive.It removes and contains in tobacco
There is protein, outside carbohydrate, medical value ingredient also important containing Salanesol, nicotine etc., exploitation prospect is wide.
Salanesol is a kind of higher effective medicinal components of added value, has the pharmacological actions such as antibacterial, anti-inflammatory and hemostasis, together
When be also synthesize farnoquinone and Co-Q10 necessary raw material.Co-Q10 has unique treatment in terms for the treatment of cardiovascular disease
Effect has significant curative effect in terms for the treatment of scurvy, duodenal ulcer and gastric ulcer, gangrenosum acne periodontitis, virus hepatitis, and
More find that it has significant auxiliary curative effect to AIDS recently.Therefore as Co-Q10 must the Salanesol of synthesis material mention
It takes, purify and also have attracted more and more attention from people.
Chlorogenic acid is a kind of important bioactive substance, have antibacterial, it is antiviral, increase white blood cell, be Hepatoprotective cholagogue, anti-
Tumour, removes the effects of free radical and stimulating central nervous system system at lowering blood pressure and blood fat.
Nicotine is a kind of alkaloid in tobacco leaf, very widely used, and purposes mainly includes that pesticide and medicine two are generous
Face.Nicotine series pesticide platymiscium insecticide, have the function of steam smoke, stomach toxicity, tag and rapidly degradation noresidue the characteristics of, extensively
Insecticide as crops such as grain, oil plant, veterinary antibiotics, herbages is ideal efficient green insecticide and biological agriculture
Medicine.In addition, high purity nicotine is to develop the special type of the drugs of illness such as treatment angiocarpy, skin, snakebite and bugbite on medical industry
Raw material.Tobacco flavor material rich in tobacco, these flavor components are mostly low pole substances, and wherein neophytadiene is cigarette
Non-pigmented terpenoid in grass, the content highest in tobacco volatile matter fragrance matter, be flavor matter important in tobacco leaf it
One.
Currently, it is more for waste tobacco leaf comprehensive utilizating research document, but it is substantially at laboratory stage.It is industrial right
The comprehensive utilization product type of waste tobacco leaf is single, mainly tobacco extract, nicotine and fertilizer kind product.Technology mostly use water and
Ethanol solution extraction, technology more fall behind, and tables of equipment one, recovery rate is low, lacks the waste tobacco leaf comprehensive production technology of scale.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above, provide a kind of utilization waste tobacco leaf recycling side
Method extracts and separates simultaneously nicotine, chlorogenic acid, Salanesol and neophytadiene, bacterial manure, scale production process from waste tobacco leaf
Route fully utilizes the effective component in waste tobacco leaf, and product category is abundant, and economic value is high, and equipment suitability is good.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows:
A kind of waste tobacco leaf recoverying and utilizing method, includes the following steps:
(1) it extracts: using waste tobacco leaf as raw material, ethanol solution is added, water bath reflux method extracts to obtain concentrate, mistake
Filter to obtain waste residue；Remaining waste residue is added into ethyl alcohol, is repeated the above steps, the extracting solution of acquisition is concentrated and is recycled ethyl alcohol,
Obtain being concentrated just cream；
(2) prepared by Salanesol: just cream will be concentrated and use sulfuric acid tune pH, extractant is added and is extracted, it is molten to merge extraction
Agent obtains extract liquor I and raffinate I；Solanesol extract will be obtained after the concentration distillation of extract liquor I, is carried out after Salanesol is saponified
Chromatography, obtains Salanesol fine work, fine work is dissolved in recrystallisation solvent, decrease temperature crystalline obtains Salanesol product；
(3) prepared by neophytadiene: loading efflux when collecting Salanesol chromatography, after efflux concentration, extraction, distillation to obtain the final product
To neophytadiene；
(4) prepared by chlorogenic acid: raffinate I being extracted with extractant, merges extraction phase solvent and is concentrated after distillation to obtain the final product
To chlorogenic acid medicinal extract, remaining as raffinate II, the water-soluble rear chromatography of chlorogenic acid medicinal extract is obtained into chlorogenic acid product；
(5) prepared by nicotine: raffinate II being used sodium hydroxide tune pH, extractant extraction is added, merges extraction and mixes
Agent simultaneously obtains cream at the beginning of nicotine after distillation is concentrated, and is stripped to obtain nicotine fine work using sulfuric acid water；
(6) prepared by organic fertilizer: the addition microorganism of waste residue obtained in step (1) being fermented, organic fertilizer is obtained.
Preferably, step (1) concentration of alcohol is 50-95%.
Preferably, step (1) extraction time is 1-5 times, extracts 0.5-2h every time.
Preferably, just cream density is 0.9-1.2g/cm for step (1) described concentration3。
Preferably, the extractant is ethyl acetate, chloroform, petroleum ether, any one in acetone.
Preferably, the recrystallisation solvent is methanol, ethyl alcohol, ethyl acetate, acetone, any one in acetonitrile.
Compared with prior art the beneficial effects of the present invention are:
The method of the present invention fully utilizes the effective component in waste tobacco leaf by being recycled to waste tobacco leaf,
The joint production process of Salanesol, neophytadiene, chlorogenic acid and nicotine is obtained, product category is abundant, and economic value is high, equipment suitability
It is good, and processing step is easy to operate, yield is high, obtains eggplant by industrial most common some equipment and operation, separated in synchronization
Five Buddhist nun's alcohol, neophytadiene, chlorogenic acid, nicotine and organic fertilizer products, environmentally friendly, no poisonous and harmful substance discharge.
Salanesol proposed by the present invention, neophytadiene, chlorogenic acid and nicotine joint production process, Salanesol purity is reachable
95% or more, yield 50%-60%, 10% or more neophytadiene purity, yield 85%, chlorogenic acid purity up to 50% or more,
Yield 85%, nicotine purity is up to 95% or more, yield 50%-60%.Product yield is higher, and purity can directly meet market
Demand.
Detailed description of the invention
Fig. 1 is process flow chart of the invention
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing.It should be noted that for
The explanation of these embodiments is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, disclosed below
The each embodiment of the present invention involved in technical characteristic can be combined with each other as long as they do not conflict with each other.
Embodiment 1
A kind of waste tobacco leaf recoverying and utilizing method, includes the following steps:
(1) it extracts: waste tobacco leaf is placed in extractor, 90% industrial alcohol is added, is heated to 70 DEG C, the duration
30min collects extracting solution, is pumped into concentration tank；Remaining waste residue is added into 90% industrial alcohol, is repeated the above steps；It will obtain
Extracting solution be concentrated and recycled ethyl alcohol, concentration tank vacuum negative pressure is 1.0Mpa, and temperature is 60 DEG C, and being concentrated into density is
1.0g/cm3g/cm3, obtain being concentrated just cream；
(2) prepared by Salanesol:
A, just cream will be concentrated to be pumped into reaction kettle, 20% aqueous sulfuric acid is added and adjusts PH to 3, according to concentrate and petroleum
Ether mass ratio is 1:1, and the petroleum ether and stirring 15min of the quality such as addition is extracted, stood 10min, extract liquor is pumped into concentration
Tank；
B, extract liquor is concentrated to and is recycled petroleum ether, remaining as raffinate I, concentrated tank pressure 1.0Mpa, temperature
It is 60 DEG C, being concentrated into density is 1.0g/cm3, obtain Salanesol crude product；
C, 90% ethyl alcohol is added according to volume ratio 1:50 in Salanesol crude product, is placed in concentration tank, adds certain mass
Sodium hydroxide, make the concentration 0.3mol/L of whole system sodium hydroxide, be heated to 70 DEG C, be saponified 30min, carried out after saponification
It is concentrated and recycles ethyl alcohol, concentrated tank pressure 1.0Mpa is concentrated into temperature in tank and reaches 60 DEG C, obtains the saponification of Salanesol crude product
Liquid；
D, Salanesol crude product saponification liquor is pumped into reaction kettle, is that petroleum ether extraction is added three times in 1:1 according to mass ratio, extraction
Liquid pump enters concentration tank, is concentrated and is recycled petroleum ether, obtains Salanesol crude product saponification medicinal extract；
E, Salanesol crude product saponification medicinal extract is dissolved in 90% ethyl alcohol according to 20g/L, 20% aqueous sulfuric acid is added and adjusts
PH to 3 is taken upper layer clear solution, is chromatographed using resin after filtering；Resin is rinsed with 95% ethanol solution, collection contains eggplant
The component of Buddhist nun's alcohol is simultaneously pumped into concentration tank and is concentrated and recycles ethyl alcohol, and concentration tank negative pressure of vacuum 1.0Mpa, temperature is 60 DEG C, concentration
It is 0.8g/cm to density3, obtain the quasi- fine work of Salanesol；
F, the quasi- fine work of Salanesol is placed in reaction kettle, is dissolved in acetonitrile according to 10g/L, be heated to 70 DEG C of dissolution 30min；It will be anti-
It answers kettle to be cooled to -20 DEG C of crystallization 5h, crystal is dried in vacuo, Salanesol fine work is obtained；
(3) prepared by neophytadiene: the ethanol solution for flowing out resin is pumped into concentration tank and is concentrated and is recycled ethyl alcohol, remaining molten
Petroleum ether extraction is added twice in the quality such as liquid, obtains neophytadiene crude product after recycling petroleum ether；
(4) prepared by chlorogenic acid:
A, it is that 1:1 stirring 15min is extracted with ethyl acetate mass ratio according to concentrate by raffinate I, stands 10min
Afterwards, extract liquor is pumped into concentration tank；It repeats the above steps, extract liquor twice is concentrated and is recycled ethyl acetate, it is remaining
For raffinate II, concentration tank vacuum negative pressure 1.0Mpa, temperature is 60 DEG C, and being concentrated into density is 0.90g/cm3, obtain chlorogenic acid
Crude product；
B, chlorogenic acid crude product is placed in reaction kettle, water is added and is dissolved, 20% aqueous sulfuric acid is added and adjusts PH to 3,
15min is stirred, 15min is stood；
C, the chlorogenic acid aqueous solution of phase lower in reaction kettle is rinsed into resin, is chromatographed, the chlorogenic acid water of resin will be flowed out
Solution is pumped into concentration tank, rinses resin with 30% ethanol solution, the chlorogenic acid ethanol solution for flowing out resin is pumped into concentration tank
In mixed and be concentrated with above-mentioned chlorogenic acid aqueous solution, concentration tank negative pressure of vacuum
1.0Mpa, temperature are 60 DEG C, and concentration obtains chlorogenic acid fine work；
(5) prepared by nicotine:
E, 20% sodium hydrate aqueous solution of raffinate II is adjusted into pH to 8, is according to concentrate and petroleum ether mass ratio
The petroleum ether and stirring 15min of 1:1, the quality such as addition are extracted, and after standing 15min, extract liquor is pumped into concentration tank；
F, raffinate is added etc. to the petroleum ether of quality, stirring 15min is extracted, after standing 15min, by extract liquor
It is pumped into concentration tank；Concentration tank negative pressure of vacuum 1.0Mpa, temperature are 50 DEG C, and being concentrated into density is 0.8g/cm3, obtain nicotine crude product；
G, nicotine crude product is placed in reaction kettle, be added water dissolution, be added 20% aqueous sulfuric acid adjust PH to 5 hereinafter,
The petroleum ether extraction of the quality such as addition is pumped into concentration tank recycling petroleum ether；
H, 20% sodium hydrate aqueous solution of the raffinate of above-mentioned steps is adjusted into pH to 8, the petroleum ether of the quality such as addition
Extract liquor is pumped into concentration tank and is concentrated and is recycled petroleum ether, concentrated tank pressure 1.0Mpa by extraction, and temperature is 60 DEG C, dense
Contracting, obtains the quasi- fine work of nicotine, and anhydrous sodium sulfate is added in the quasi- fine work of nicotine, is dehydrated, obtains nicotine fine work；
(6) prepared by organic fertilizer: the addition microorganism of waste residue obtained in step (1) being fermented, organic fertilizer is obtained.
Embodiment 2
A kind of waste tobacco leaf recoverying and utilizing method, includes the following steps:
(1) it extracts: waste tobacco leaf is placed in extractor, 90% industrial alcohol is added, is heated to 70 DEG C, the duration
40min collects extracting solution, is pumped into concentration tank；Remaining waste residue is added into 90% industrial alcohol, is repeated the above steps；In repetition
Step to be stated, the extracting solution of acquisition is concentrated and is recycled ethyl alcohol, concentration tank vacuum negative pressure is 1.0Mpa, and temperature is 60 DEG C,
Being concentrated into density is 1.2g/cm3, obtain being concentrated just cream；
(2) prepared by Salanesol:
A, just cream will be concentrated to be pumped into reaction kettle, 30% aqueous sulfuric acid is added and adjusts pH to 2, the petroleum of the quality such as addition
Ether stirring 20min is extracted, and stands 10min, extract liquor is pumped into concentration tank；
B, extract liquor is concentrated to and is recycled petroleum ether, remaining as raffinate I, concentrated tank pressure 1.0Mpa, temperature
It is 60 DEG C, being concentrated into density is 1.2g/cm3, obtain Salanesol crude product；
C, 90% ethyl alcohol is added according to volume ratio 1:50 in Salanesol crude product, is placed in concentration tank, adds certain mass
Sodium hydroxide, make the concentration 0.3mol/L of whole system sodium hydroxide, be heated to 70 DEG C, be saponified 30min, carried out after saponification
It is concentrated and recycles ethyl alcohol, concentrated tank pressure 1.0Mpa is concentrated into temperature in tank and reaches 60 DEG C, obtains the saponification of Salanesol crude product
Liquid；
D, Salanesol crude product saponification liquor is pumped into reaction kettle, is that petroleum ether extraction is added three times in 1:1 according to mass ratio, extraction
Liquid pump enters concentration tank, is concentrated and is recycled petroleum ether, obtains Salanesol crude product saponification medicinal extract；
E, Salanesol crude product saponification medicinal extract is dissolved in 90% ethyl alcohol according to 20g/L, 20% aqueous sulfuric acid is added and adjusts
PH to 2 is taken upper layer clear solution, is chromatographed using resin after filtering；Resin is rinsed with 95% ethanol solution, collection contains eggplant
The component of Buddhist nun's alcohol is simultaneously pumped into concentration tank and is concentrated and recycles ethyl alcohol, and concentration tank negative pressure of vacuum 1.0Mpa, temperature is 60 DEG C, concentration
It is 1.0g/cm to density3, obtain the quasi- fine work of Salanesol；
F, the quasi- fine work of Salanesol is placed in reaction kettle, is dissolved in acetonitrile according to 10g/L, be heated to 75 DEG C of dissolution 30min；It will be anti-
It answers kettle to be cooled to -20 DEG C of crystallization 8h, crystal is dried in vacuo, Salanesol fine work is obtained；
(3) prepared by neophytadiene: the ethanol solution for flowing out resin is pumped into concentration tank and is concentrated and is recycled ethyl alcohol, remaining molten
Petroleum ether extraction is added twice in the quality such as liquid, obtains neophytadiene crude product after recycling petroleum ether；
(4) prepared by chlorogenic acid:
It a, is 1:1, the ethyl acetate stirring of the quality such as addition according to concentrate and ethyl acetate mass ratio by raffinate I
20min is extracted, and after standing 10min, extract liquor is pumped into concentration tank；It repeats the above steps, extract liquor twice is carried out
It is concentrated and recycles ethyl acetate, remaining as raffinate II, concentration tank vacuum negative pressure 1.0Mpa, temperature is 60 DEG C, is concentrated into close
Degree is 1.0g/cm3, obtain chlorogenic acid crude product；
B, chlorogenic acid crude product is placed in reaction kettle, water is added and is dissolved, 25% aqueous sulfuric acid is added and adjusts pH to 2,
20min is stirred, 15min is stood；
C, resin will be rinsed by the chlorogenic acid aqueous solution of lower phase in reaction kettle, be chromatographed, after will flow out the chlorogenic acid of resin
Aqueous solution is pumped into concentration tank, rinses resin with 30% ethanol solution, the chlorogenic acid ethanol solution for flowing out resin is pumped into concentration
It is mixed and is concentrated with above-mentioned chlorogenic acid aqueous solution in tank, concentration tank negative pressure of vacuum 1.0Mpa, temperature is 60 DEG C, and concentration obtains
To chlorogenic acid fine work；
(5) prepared by nicotine:
E, 20% sodium hydrate aqueous solution of raffinate II is adjusted into pH to 10, is according to concentrate and petroleum ether mass ratio
The petroleum ether and stirring 20min of 1:1, the quality such as addition are extracted, and after standing 15min, extract liquor is pumped into concentration tank；
F, by raffinate add according to concentrate and petroleum ether mass ratio be 1:1 etc. quality petroleum ether, stirring
20min is extracted, and after standing 15min, extract liquor is pumped into concentration tank；Concentration tank negative pressure of vacuum 1.0Mpa, temperature are 50 DEG C,
Being concentrated into density is 1.0g/cm3, obtain nicotine crude product；
G, nicotine crude product is placed in reaction kettle, be added water dissolution, be added 20% aqueous sulfuric acid adjust pH to 3 hereinafter,
The petroleum ether extraction of the quality such as addition is pumped into concentration tank recycling petroleum ether；
H, 20% sodium hydrate aqueous solution of the raffinate of above-mentioned steps is adjusted into pH to 10, the petroleum ether of the quality such as addition
Extract liquor is pumped into concentration tank and is concentrated and is recycled petroleum ether, concentrated tank pressure 1.0Mpa by extraction, and temperature is 60 DEG C, dense
Contracting, obtains the quasi- fine work of nicotine, and anhydrous sodium sulfate is added in the quasi- fine work of nicotine, is dehydrated, obtains nicotine fine work；
(6) prepared by organic fertilizer: the addition microorganism of waste residue obtained in step (1) being fermented, organic fertilizer is obtained.
Embodiment 3
A kind of waste tobacco leaf recoverying and utilizing method, includes the following steps:
(1) it extracts: waste tobacco leaf is placed in extractor, 90% industrial alcohol is added, is heated to 70 DEG C, the duration
60min collects extracting solution, is pumped into concentration tank；Remaining waste residue is added into 90% industrial alcohol, is repeated the above steps；In repetition
Step to be stated, the extracting solution of acquisition is concentrated and is recycled ethyl alcohol, concentration tank vacuum negative pressure is 1.0Mpa, and temperature is 60 DEG C,
Being concentrated into density is 1.2g/cm3, obtain being concentrated just cream；
(2) prepared by Salanesol:
A, just cream will be concentrated to be pumped into reaction kettle, 40% aqueous sulfuric acid is added and adjusts pH to 1, according to concentrate and petroleum
Ether mass ratio is 1:1, and the petroleum ether and stirring 30min of the quality such as addition is extracted, stood 10min, extract liquor is pumped into concentration
Tank；
B, extract liquor is concentrated to and is recycled petroleum ether, remaining as raffinate I, concentrated tank pressure 1.0Mpa, temperature
It is 60 DEG C, being concentrated into density is 1.2g/cm3, obtain Salanesol crude product；
C, 90% ethyl alcohol is added according to volume ratio 1:50 in Salanesol crude product, is placed in concentration tank, adds certain mass
Sodium hydroxide, make the concentration 0.3mol/L of whole system sodium hydroxide, be heated to 70 DEG C, be saponified 30min, carried out after saponification
It is concentrated and recycles ethyl alcohol, concentrated tank pressure 1.0Mpa is concentrated into temperature in tank and reaches 60 DEG C, obtains the saponification of Salanesol crude product
Liquid；
D, Salanesol crude product saponification liquor is pumped into reaction kettle, is that petroleum ether extraction is added three times in 1:1 according to mass ratio, extraction
Liquid pump enters concentration tank, is concentrated and is recycled petroleum ether, obtains Salanesol crude product saponification medicinal extract；
E, Salanesol crude product saponification medicinal extract is dissolved in 90% ethyl alcohol according to 20g/L, 20% aqueous sulfuric acid is added and adjusts
PH to 1-3 is taken upper layer clear solution, is chromatographed using resin after filtering；Resin is rinsed with 95% ethanol solution, collection contains
The component of Salanesol is simultaneously pumped into concentration tank and is concentrated and is recycled ethyl alcohol, and concentration tank negative pressure of vacuum 1.0Mpa, temperature is 60 DEG C, dense
Being reduced to density is 1.0g/cm3, obtain the quasi- fine work of Salanesol；
F, the quasi- fine work of Salanesol is placed in reaction kettle, is dissolved in acetonitrile according to 10g/L, be heated to 80 DEG C of dissolution 30min；It will be anti-
It answers kettle to be cooled to -20 DEG C of crystallization 10h, crystal is dried in vacuo, Salanesol fine work is obtained；
(3) prepared by neophytadiene: the ethanol solution for flowing out resin is pumped into concentration tank and is concentrated and is recycled ethyl alcohol, remaining molten
Petroleum ether extraction is added twice in the quality such as liquid, obtains neophytadiene crude product after recycling petroleum ether；
(4) prepared by chlorogenic acid:
It a, is 1:1, the ethyl acetate stirring of the quality such as addition according to concentrate and ethyl acetate mass ratio by raffinate I
30min is extracted, and after standing 10min, extract liquor is pumped into concentration tank；It repeats the above steps, extract liquor twice is carried out
It is concentrated and recycles ethyl acetate, remaining as raffinate II, concentration tank vacuum negative pressure 1.0Mpa, temperature is 60 DEG C, is concentrated into close
Degree is 1.1g/cm3, obtain chlorogenic acid crude product；
B, chlorogenic acid crude product is placed in reaction kettle, water is added and is dissolved, 30% aqueous sulfuric acid is added and adjusts pH to 3,
30min is stirred, 15min is stood；
C, resin will be rinsed by the chlorogenic acid aqueous solution of lower phase in reaction kettle, be chromatographed, after will flow out the chlorogenic acid of resin
Aqueous solution is pumped into concentration tank, rinses resin with 30% ethanol solution, the chlorogenic acid ethanol solution for flowing out resin is pumped into concentration
It is mixed and is concentrated with above-mentioned chlorogenic acid aqueous solution in tank, concentration tank negative pressure of vacuum 1.0Mpa, temperature is 60 DEG C, and concentration obtains
To chlorogenic acid fine work；
(5) prepared by nicotine:
E, 20% sodium hydrate aqueous solution of raffinate II is adjusted into pH to 12, is according to concentrate and petroleum ether mass ratio
The petroleum ether and stirring 30min of 1:1, the quality such as addition are extracted, and after standing 15min, extract liquor is pumped into concentration tank；
F, by raffinate add according to concentrate and petroleum ether mass ratio be 1:1 etc. quality petroleum ether, stirring
30min is extracted, and after standing 15min, extract liquor is pumped into concentration tank；Concentration tank negative pressure of vacuum 1.0Mpa, temperature are 50 DEG C,
Being concentrated into density is 1.0g/cm3, obtain nicotine crude product；
G, nicotine crude product is placed in reaction kettle, be added water dissolution, be added 20% aqueous sulfuric acid adjust pH to 5 hereinafter,
The petroleum ether extraction of the quality such as addition is pumped into concentration tank recycling petroleum ether；
H, 20% sodium hydrate aqueous solution of the raffinate of above-mentioned steps is adjusted into PH to 12, the petroleum ether of the quality such as addition
Extract liquor is pumped into concentration tank and is concentrated and is recycled petroleum ether, concentrated tank pressure 1.0Mpa by extraction, and temperature is 60 DEG C, dense
Contracting, obtains the quasi- fine work of nicotine, and anhydrous sodium sulfate is added in the quasi- fine work of nicotine, is dehydrated, obtains nicotine fine work；
(6) prepared by organic fertilizer: the addition microorganism of waste residue obtained in step (1) being fermented, organic fertilizer is obtained.
The above are present pre-ferred embodiments, it is only applicable to the principle for helping to understand the embodiment of the present invention；Meanwhile for this
The those skilled in the art in field, according to the present embodiment, there will be changes in terms of specific embodiments and scope of application, comprehensive
Upper described, the contents of this specification are not to be construed as limiting the invention.
Claims (6)
1. a kind of waste tobacco leaf recoverying and utilizing method, characterized by the following steps:
(1) it extracts: using waste tobacco leaf as raw material, ethanol solution is added, water bath reflux method extracts to obtain concentrate, filters
Waste residue；Remaining waste residue is added into ethyl alcohol, is repeated the above steps, the extracting solution of acquisition is concentrated and is recycled ethyl alcohol, is obtained
Just cream is concentrated；
(2) prepared by Salanesol: just cream will be concentrated and use sulfuric acid tune pH, extractant is added and is extracted, merges extractant and obtains
To extract liquor I and raffinate I；Solanesol extract will be obtained after the concentration distillation of extract liquor I, carries out layer after Salanesol is saponified
Analysis, obtains Salanesol fine work, fine work is dissolved in recrystallisation solvent, decrease temperature crystalline obtains Salanesol product；
(3) prepared by neophytadiene: loading efflux when collecting Salanesol chromatography obtains new after efflux concentration, extraction, distillation
Phytadiene；
(4) chlorogenic acid prepare: raffinate I is extracted with extractant, merge extraction phase solvent and be concentrated distillation after obtain it is green
The water-soluble rear chromatography of chlorogenic acid medicinal extract is obtained chlorogenic acid product remaining as raffinate II by ortho acid medicinal extract；
(5) prepared by nicotine: raffinate II being used sodium hydroxide tune pH, extractant extraction is added, merges extraction phase solvent simultaneously
Nicotine just cream is obtained after concentration distillation, is stripped to obtain nicotine fine work using sulfuric acid water；
(6) prepared by organic fertilizer: the addition microorganism of waste residue obtained in step (1) being fermented, organic fertilizer is obtained.
2. waste tobacco leaf recoverying and utilizing method according to claim 1, it is characterised in that: step (1) described concentration of alcohol
For 50-95%.
3. waste tobacco leaf recoverying and utilizing method according to claim 1, it is characterised in that: step (1) described extraction time
It is 1-5 times, extracts 0.5-2h every time.
4. waste tobacco leaf recoverying and utilizing method according to claim 1, it is characterised in that: the first cream of step (1) described concentration
Density is 0.9-1.2g/cm3。
5. waste tobacco leaf recoverying and utilizing method according to claim 1, it is characterised in that: the extractant is acetic acid second
Ester, chloroform, petroleum ether, any one in acetone.
6. waste tobacco leaf recoverying and utilizing method according to claim 1, it is characterised in that: the recrystallisation solvent be methanol,
Ethyl alcohol, ethyl acetate, acetone, any one in acetonitrile.
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| CN110041303A (en) * | 2019-05-30 | 2019-07-23 | 深圳波顿香料有限公司 | The process of neophytadiene, carotenoid and nicotine is extracted from waste tobacco |
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