CN102731475A - Method for recycling nicotine and hemicellulose in tobacco waste - Google Patents
Method for recycling nicotine and hemicellulose in tobacco waste Download PDFInfo
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- CN102731475A CN102731475A CN2012100425568A CN201210042556A CN102731475A CN 102731475 A CN102731475 A CN 102731475A CN 2012100425568 A CN2012100425568 A CN 2012100425568A CN 201210042556 A CN201210042556 A CN 201210042556A CN 102731475 A CN102731475 A CN 102731475A
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Abstract
The invention relates a chemical extraction method of agricultural waste, particularly a method for recycling nicotine and hemicellulose in tobacco waste, comprising the following steps: crushing the tobacco waste, adding 10-30 times volume of water, regulating the pH value to 11-13, processing under microwave to obtain a pretreatment material; filtering the pretreatment material obtained by the above step, taking the filtrate, and adding sulfuric acid in the filtrate; conducting fully reacting on the mixed solution to obtain nicotine sulfate and then to obtain nicotine, wherein the residues are used for extracting hemicellulose, cellulose and lignin. The extraction process can respectively process the filtrate and the filter residues in the pretreatment liquid, nicotine and hemicellulose can be extracted from the filtrate, and lignin and cellulose can be extracted from the filter residues. The method is ingenious, green and practical, can be used for realizing large-scale industrial production.
Description
Technical field
The present invention relates to the chemical extraction field, particularly the chemical extraction method of agricultural waste.
Background technology
China is tobacco big producing country, not only in the process of the accumulating of tobacco leaf and production of cigarettes, produce a large amount of scrap, scarp, offal, pollute or tobacco waste such as the tobacco leaf that goes mouldy, and the tobacco grower to abandon every year in the quantity of the discarded tobacco leaf in field also be considerable.Contain the multiple chemical ingredients that the value utilized is arranged in the tobacco leaf,, then not only improved the pollution of waste, created wealth for country again simultaneously environment if it is fully utilized.But because state-of-the-art falls behind, product cost is higher and cause the situation that the market competitiveness is not high, comprehensive utilization ratio is low.
Summary of the invention
The invention provides a kind of from tobacco the continuous novel method of extraction nicotine, semicellulose product.This method extraction nicotine foundation is under alkaline condition, to utilize microwave technology; Smudge cells material to greatest extent; Obtain more nicotine products, remaining filter residue is used to extract semicellulose, xylogen, Mierocrystalline cellulose, reach the purpose of the comprehensive utilization of tobacco.
For reaching above purpose, its technical scheme comprises:
Utilize method again in the tobacco waste, specifically may further comprise the steps:
The A raw materials pretreatment
Tobacco waste is pulverized, added and be equivalent to 10-30 times of water of tobacco waste volume, adjustment pH value is 11-13, in microwave treatment, gets the pre-treatment material; The purpose of microwave treatment is the smudge cells material, and the destructiveness of cellular material is big more, and the yield of nicotine products is proportionate to a certain extent.
The extraction of B nicotine sulfate
Steps A gained pre-treatment material is filtered, get filtrating, in filtrating, add sulfuric acid, get mixed solution; After liquid to be mixed fully reacts, get nicotine sulfate, said vitriolic massfraction is 5-15%, and temperature of reaction is 80-140 ℃.
Present method is except extraction nicotine/nicotine sulfate, can also further utilize residuum to extract other products, like semicellulose, the steps include: the residual solution behind the extraction nicotine is regulated the pH value to 3.0-5.0, and centrifugal, residue is semicellulose A.Semicellulose A refers to that mainly adopting alkali extracting solution is semicellulose A with the part of acetic acid neutralization precipitation.
Further, the residual solution behind the extraction nicotine is regulated the pH value to 3.0-5.0, centrifugal, residue is semicellulose A, and the suspension-s after centrifugal is with ethanol precipitating, centrifugal, and residue is a hemicellulose B.Hemicellulose B refers to that mainly supernatant is a hemicellulose B with the part of ethanol sedimentation.
The difference of semicellulose A and B is: removing the material beyond the pectin substance among the polysaccharide crowd of matter gel between between plant cell wall formation Mierocrystalline cellulose O-fiber, is the staple that constitutes primary wall.Comprise glucose, wood sugar, seminose, pectinose and semi-lactosi etc.; Be connected with covalent linkage, hydrogen bond, ehter bond and ester bond respectively between the monose polymer; They and formations such as extensin, other structural protein, wall enzyme, Mierocrystalline cellulose and pectin have certain degree of hardness and elastic cell walls, thereby present stable chemical structure.Be originally from the total fiber element with 17.5%NaOH so that the general name of the polysaccharide component that 24%KOH extracts, and do not have corresponding specific chemical structure.Alkali extracting solution is semicellulose A with the part of acetic acid neutralization precipitation, and supernatant is a hemicellulose B with the part of ethanol sedimentation.As important polysaccharide except that neutral polysaccharides such as xylan, VISOSE, araboxylan, glucomannan, arabogalactan.
In the steps A, be that microwave treatment is no less than 20min under the 200W condition wherein at power; Or be that microwave treatment is no less than 10min under the 300W condition at power; Or be that microwave treatment is no less than 1min under the 600W condition at power.
Wherein, in the steps A, the particle diameter of said tobacco waste is not more than 10 orders.
Wherein, among the step B, adopt distillation and extraction method to extract nicotine sulfate.
Wherein, said nicotine sulfate solution is extracted, get nicotine with normal hexane.
Wherein, with the residual solution behind the extraction nicotine with the salt acid for adjusting pH value to 3.0-5.0, centrifugal.
Wherein, it is that 95% ethanol precipitating is no less than 30 minutes, centrifugally under the 1000r/min condition is no less than 5 minutes that the suspension-s after centrifugal uses volumetric concentration, and residue is a hemicellulose B.
This technology is except being used for tobacco waste to distinguish extraction nicotine and the semicellulose, and another benefit is: also can after steps A is accomplished, the gained filter residue be carried out xylogen and cellulosic extraction synchronously.
Concrete scheme is:
The A raw materials pretreatment
Tobacco waste is pulverized, added and be equivalent to tobacco waste 10-30 times water, adjustment pH value be 11-13, is that processing is no less than 1 minute under the microwave of 100W at power, must the pre-treatment material;
The extraction of B xylogen
Steps A gained pre-treatment material is filtered, and filter residue uses acid for adjusting pH value to be 4.0-5.0, and reaction was not less than 40 minutes, and with ionic liquid 1-butyl-abundant solubilizing reaction of 3-Methylimidazole villaumite, solid-liquid separation gets liquid and solid, and said solid is an xylogen.
Wherein,, must precipitate adding deionized water in the step B gained liquid, the said Mierocrystalline cellulose that is precipitated as, the mass ratio of said Mierocrystalline cellulose and said ionic liquid 1-butyl-3-Methylimidazole villaumite is 1: 6～1: 20.
Wherein, the gained Mierocrystalline cellulose is used cold water flush, suction filtration also carries out vacuum-drying, and drying temperature is 70～100 ℃, and be 10～12 hours time of drying.
Wherein, said solubilizing reaction carries out under whipped state, and the reaction times is 30～240 minutes.
Wherein, among the step B, the mode of said solid-liquid separation is specially spinning, and the centrifugal time is 5～8 minutes, and centrifugal speed is 1500～4000 rev/mins.
Wherein, in step B, steps A gained pre-treatment material is filtered, filter residue uses acid for adjusting pH value to be 4.0-5.0, and reaction is 60 minutes under 70-95 ℃ of condition, cooling.
Wherein, in step B, the temperature of solubilizing reaction is 70-95 ℃, and the time of reaction is 4 hours.
This extraction process can be handled filtrating in the pretreatment fluid and filter residue respectively, but extraction nicotine and semicellulose in the filtrating can extract xylogen and Mierocrystalline cellulose in the filter residue.This programme design is ingenious, and environmental protection is practical, can realize suitability for industrialized production on a large scale.
Embodiment
The tobacco waste of indication has another name called tobacco leftovers among the present invention, is specially: useless time tobacco leaf, offal.Low in a large number, hypo-tobacco leaf and cigarette tankage, tobacco waste is a large amount of sub products that produce in the production of cigarettes, is rich in various organic compositions and secondary metabolite.Tobacco waste also can be made material substitution with tobacco.
Tobacco waste among the following embodiment comes from Chongqing silver good fortune biological organic fertilizer ltd, and its water cut accounts for 7% of tobacco waste total mass.
Among the following embodiment, cellulosic purity is meant cellulosic yield.
Cellulosic method for detecting purity is the nitric acid Ethanol Method.Xylogen, the detection method of semicellulose purity are the normal form fibre method.In addition, adopt ionic liquid 1-butyl-3-Methylimidazole villaumite to extract cellulosic detailed protocol, see application number for details and be 201110248519.8 one Chinese patent application.
Embodiment 1
With 20 order 100g tobacco waste powder, add after the oven dry impurity elimination and be equivalent to 10 times of normal-temperature water of tobacco waste volume, adjustment pH value is 11; Under microwave power 200W, behind the microwave 20min, filter; It is that 10% sulfuric acid carries out distillation extraction as solvent that filtrating is used massfraction; Distillation temperature is 100 ℃, gets the product nicotine sulfate, obtains natural nicotine 3.2g with n-hexane extraction then; It is 3.0 that residual filtrate uses HCL to regulate filtrating pH value, and centrifugal (centrifugal 10min under the 1500r/min condition) gets semicellulose A8.6g; Suspension-s after centrifugal gets hemicellulose B 4.2g with the ethanol precipitating of volume(tric)fraction 95%, centrifugal (centrifugal 10min under the 2000r/min condition).
Filter residue after the filtration of steps A gained pre-treatment material is carried out the extraction of xylogen synchronously, be specially: it is 4.0 that filter residue uses 0.3mol/l HCL to regulate the pH value, is heated to 75 ℃ of reactions 1 hour, and cooling, filtration contain xylogen and Mierocrystalline cellulose in the filtering filter residue.With filter residue adopt ionic liquid 1-butyl-3-Methylimidazole villaumite be heated to 80 ℃ the reaction 4h after, separate solid and liquid, solid is an xylogen, adds deionized water in the liquid immediately and obtains Mierocrystalline cellulose, and under 80 ℃ of conditions, be put in dry 12h in the vacuum drying oven.
Can get through analyzing, semicellulose is 12.8g, and purity is 85.3%; Mierocrystalline cellulose is 28.5g, and purity (yield) is 86.4%; Xylogen is 5.4g, and purity is 77.1%.
Embodiment 2
With 20 orders grass waste powder, add after the oven dry impurity elimination and be equivalent to 10 times of normal-temperature water of tobacco waste volume, adjustment pH value is 11; Under microwave power 400W, behind the microwave 30min, filter; It is that 10% sulfuric acid carries out distillation extraction as solvent that filtrating is used massfraction; Distillation temperature is 100 ℃, gets the product nicotine sulfate, obtains natural nicotine 3.6g with n-hexane extraction then; It is 4.0 that residual filtrate uses HCL to regulate filtrating pH value, centrifugal (centrifugal 10min under the 1500r/min condition), and getting semicellulose A is 8.8g; Suspension-s after centrifugal gets hemicellulose B 4.7g with centrifugal 10min under 95% ethanol precipitating, the centrifugal 2000r/min condition.
Filter residue after the filtration of steps A gained pre-treatment material is carried out the extraction of xylogen synchronously, be specially: it is 5.0 that filter residue uses 0.3mol/lHCL to regulate the pH value, is heated to 75 ℃ of reactions 1 hour, and cooling, filtration contain xylogen and Mierocrystalline cellulose in the filtering filter residue.With filter residue adopt ionic liquid 1-butyl-3-Methylimidazole villaumite be heated to 80 ℃ the reaction 4h after, separate solid and liquid, solid is an xylogen, adds deionized water in the liquid immediately and obtains Mierocrystalline cellulose, and under 80 ℃ of conditions, be put in dry 12h in the vacuum drying oven.
Can get through analyzing, semicellulose is 13.5g, and purity is 96.4%; Mierocrystalline cellulose is for being 30.2g, and purity is 91.5%; Xylogen is 6.1g, and purity is 87.1%.
Embodiment 3
With 20 order 100g grass waste powder, add after the oven dry impurity elimination and be equivalent to 10 times of normal-temperature water of tobacco waste volume, adjustment pH value is 11; Behind the effect 30min; Filter, it is that 10% sulfuric acid carries out distillation extraction as solvent that filtrating is used massfraction, and distillation temperature is 100 ℃; Get the product nicotine sulfate, use n-hexane extraction to obtain natural nicotine then and be 1.6g; It is 3.0 that residual filtrate uses HCL to regulate filtrating pH value, centrifugal (centrifugal 10min under the 1500r/min condition), and getting semicellulose A is 4.8g; Suspension-s after centrifugal is with 95% ethanol precipitating, centrifugal, and centrifugal condition is centrifugal 10min under the 2000r/min condition), hemicellulose B be 1.5g.
Filter residue after the filtration of steps A gained pre-treatment material is carried out the extraction of xylogen synchronously, be specially: it is 4.0 that filter residue uses 0.3mol/lHCL to regulate the pH value, is heated to 75 ℃ of reactions 1 hour, and cooling, filtration contain xylogen and Mierocrystalline cellulose in the filtering filter residue.With filter residue adopt ionic liquid 1-butyl-3-Methylimidazole villaumite be heated to 80 ℃ the reaction 4h after, separate solid and liquid, solid is an xylogen, adds deionized water in the liquid immediately and obtains Mierocrystalline cellulose, and under 80 ℃ of conditions, be put in dry 12h in the vacuum drying oven.
Can get through analyzing, semicellulose is 6.3g, and purity is 45.0%; Mierocrystalline cellulose is 12.3g, and purity is 37.3%; Xylogen is 2.1g, and purity is 30.0%.
Embodiment 4
With 20 order 100g tobacco waste powder, add after the oven dry impurity elimination and be equivalent to 10 times of normal-temperature water of tobacco waste volume, adjustment pH value is 7; Under microwave power 400W, behind the microwave 30min, filter; It is that 10% sulfuric acid carries out distillation extraction as solvent that filtrating is used massfraction; Distillation temperature is 100 ℃, gets the product nicotine sulfate, obtains natural nicotine 2.6g with n-hexane extraction then; It is 4.0 that residual filtrate uses HCL to regulate filtrating pH value, and centrifugal (centrifugal 10min under the 1500r/min condition) gets semicellulose A5.8g; Suspension-s after centrifugal is with 95% ethanol precipitating, centrifugal, and centrifugal condition is centrifugal 10min under the 2000r/min condition, hemicellulose B 3.7g.
Filter residue after the filtration of steps A gained pre-treatment material is carried out the extraction of xylogen synchronously, be specially: it is 5.0 that filter residue uses 0.3mol/lHCL to regulate the pH value, is heated to 75 ℃ of reactions 1 hour, and cooling, filtration contain xylogen and Mierocrystalline cellulose in the filtering filter residue.With filter residue adopt ionic liquid 1-butyl-3-Methylimidazole villaumite be heated to 80 ℃ the reaction 4h after, separate solid and liquid, solid is an xylogen, adds deionized water in the liquid immediately and obtains Mierocrystalline cellulose, and under 80 ℃ of conditions, be put in dry 12h in the vacuum drying oven.
Can get through analyzing, semicellulose is 9.5g, and purity is 67.9%; Mierocrystalline cellulose is 21.2g, and purity is 64.2%; Xylogen is 4.8g, and purity is 68.6%.
Embodiment 5
With 20 order 100g grass waste powder, add after the oven dry impurity elimination and be equivalent to 10 times of normal-temperature water of tobacco waste volume, adjustment pH value is 11; Under microwave power 400W, behind the microwave 30min, filter; It is that 10% sulfuric acid carries out distillation extraction as solvent that filtrating is used massfraction; Distillation temperature is 100 ℃, gets the product nicotine sulfate, uses n-hexane extraction to obtain natural nicotine then and is 3.6g; It is 2.0 that residual filtrate uses HCL to regulate filtrating pH value, and centrifugal (centrifugal 10min under the 1500r/min condition) gets semicellulose A5.8g; Suspension-s after centrifugal is with 95% ethanol precipitating, centrifugal, and centrifugal condition is centrifugal 10min under the 2000r/min condition, hemicellulose B 2.3g.
Filter residue after the filtration of steps A gained pre-treatment material is carried out the extraction of xylogen synchronously, be specially: it is 5.0 that filter residue uses 0.3mol/l HCL to regulate the pH value, is heated to 75 ℃ of reactions 1 hour, and cooling, filtration contain xylogen and Mierocrystalline cellulose in the filtering filter residue.With filter residue adopt ionic liquid 1-butyl-3-Methylimidazole villaumite be heated to 80 ℃ the reaction 4h after, separate solid and liquid, solid is an xylogen, adds deionized water in the liquid immediately and obtains Mierocrystalline cellulose, and under 80 ℃ of conditions, be put in dry 12h in the vacuum drying oven.
Can get through analyzing, semicellulose is 8.1g, and purity is 57.9%; Mierocrystalline cellulose is 22.4g, and purity is 67.9%; Xylogen is 5.4g, and purity is 77.1%.
Embodiment 6
With 20 order 100g grass waste powder, add after the oven dry impurity elimination and be equivalent to 30 times of normal-temperature water of tobacco waste volume, adjustment pH value is 11; Under microwave power 100W, behind the microwave 30min, filter; It is that 10% sulfuric acid carries out distillation extraction as solvent that filtrating is used massfraction; Distillation temperature is 100 ℃, gets the product nicotine sulfate, obtains natural nicotine 1.9g with n-hexane extraction then; It is 4.0 that residual filtrate uses HCL to regulate filtrating pH value, and centrifugal (centrifugal 10min under the 1500r/min condition) gets semicellulose A2.8g; Suspension-s after centrifugal is with 95% ethanol precipitating, centrifugal, and centrifugal condition is centrifugal 10min under the 2000r/min condition, hemicellulose B 2.1g.
Filter residue after the filtration of steps A gained pre-treatment material is carried out the extraction of xylogen synchronously, be specially: it is 5.0 that filter residue uses 0.3mol/l HCL to regulate the pH value, is heated to 75 ℃ of reactions 1 hour, and cooling, filtration contain xylogen and Mierocrystalline cellulose in the filtering filter residue.With filter residue adopt ionic liquid 1-butyl-3-Methylimidazole villaumite be heated to 80 ℃ the reaction 4h after, separate solid and liquid, solid is an xylogen, adds deionized water in the liquid immediately and obtains Mierocrystalline cellulose, and under 80 ℃ of conditions, be put in dry 12h in the vacuum drying oven.
Can get through analyzing, semicellulose is 4.9g, and purity is 35.0%; Mierocrystalline cellulose is 15.3g, and purity is 91.5%; Xylogen is 6.1g, and purity is 87.1%.
Explanation is at last; Above embodiment is only unrestricted in order to technical scheme of the present invention to be described; Although with reference to preferred embodiment the present invention is specified, those of ordinary skill in the art should be appreciated that and can make amendment or be equal to replacement technical scheme of the present invention; And not breaking away from the aim and the scope of technical scheme of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (9)
1. utilize method again in the tobacco waste, it is characterized in that, specifically may further comprise the steps:
The A raw materials pretreatment
Tobacco waste is pulverized, added and be equivalent to 10-30 times of water of tobacco waste volume, adjustment pH value is 11-13, in microwave treatment, gets the pre-treatment material;
The extraction of B nicotine sulfate
Steps A gained pre-treatment material is filtered, get filtrating, in filtrating, add sulfuric acid, get mixed solution; After liquid to be mixed fully reacts, get nicotine sulfate, said vitriolic massfraction is 5-15%, and temperature of reaction is 80-140 ℃.
2. utilize method again in the tobacco waste according to claim 1, it is characterized in that the residual solution behind the extraction nicotine is regulated the pH value to 3.0-5.0, and centrifugal, residue is semicellulose A.
3. utilize method again in the tobacco waste according to claim 2, it is characterized in that, the residual solution behind the extraction nicotine is regulated the pH value to 3.0-5.0; Centrifugal; Residue is semicellulose A, and the suspension-s after centrifugal is with ethanol precipitating, centrifugal, and residue is a hemicellulose B.
4. utilizing method again in the tobacco waste according to claim 1, it is characterized in that, in the steps A, is that microwave treatment is no less than 20min under the 200W condition at power; Or be that microwave treatment is no less than 10min under the 300W condition at power; Or be that microwave treatment is no less than 1min under the 600W condition at power.
5. utilize method again in the tobacco waste according to claim 1, it is characterized in that in the steps A, the particle diameter of said tobacco waste is not more than 10 orders.
6. utilize method again in the tobacco waste according to claim 1, it is characterized in that, among the step B, adopt distillation and extraction method to extract nicotine sulfate.
7. according to utilizing method again in claim 1 or the 7 described tobacco wastes, it is characterized in that, said nicotine sulfate solution extracted with normal hexane, nicotine.
8. utilize method again in the tobacco waste according to claim 2, it is characterized in that, with the residual solution behind the extraction nicotine with the salt acid for adjusting pH value to 3.0-5.0, centrifugal.
9. utilize method again in the tobacco waste according to claim 3; It is characterized in that; It is that 95% ethanol precipitating is no less than 30 minutes, centrifugally under the 1000r/min condition is no less than 5 minutes that suspension-s after centrifugal uses volumetric concentration, and residue is a hemicellulose B.
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| CN2012100425568A CN102731475A (en) | 2012-02-23 | 2012-02-23 | Method for recycling nicotine and hemicellulose in tobacco waste |
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| CN2012100425568A CN102731475A (en) | 2012-02-23 | 2012-02-23 | Method for recycling nicotine and hemicellulose in tobacco waste |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103342763A (en) * | 2013-07-11 | 2013-10-09 | 宜宾丝丽雅集团有限公司 | Method for extracting and recovering hemicellulose from squeezed waste alkali |
| CN106749172A (en) * | 2016-11-22 | 2017-05-31 | 中国烟草总公司郑州烟草研究院 | A kind of method that utilization subcritical abstraction molecular clock GC-MS purifies nicotine |
| CN108077996A (en) * | 2017-12-06 | 2018-05-29 | 湖北中烟工业有限责任公司 | One preparation method and application for growing tobacco cationic hemicellulose |
| CN108464192A (en) * | 2018-06-19 | 2018-08-31 | 贵州省贵福菌业发展有限公司 | A kind of oil tea mushroom strains activation medium |
| CN111455705A (en) * | 2020-05-25 | 2020-07-28 | 贺先佑 | Method for manufacturing corrugated paper pulp by using moldy tobacco leaves and other tobacco wastes |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342763A (en) * | 2013-07-11 | 2013-10-09 | 宜宾丝丽雅集团有限公司 | Method for extracting and recovering hemicellulose from squeezed waste alkali |
| CN103342763B (en) * | 2013-07-11 | 2015-10-28 | 宜宾丝丽雅集团有限公司 | Method for extracting and recovering hemicellulose from squeezed waste alkali |
| CN106749172A (en) * | 2016-11-22 | 2017-05-31 | 中国烟草总公司郑州烟草研究院 | A kind of method that utilization subcritical abstraction molecular clock GC-MS purifies nicotine |
| CN106749172B (en) * | 2016-11-22 | 2019-03-01 | 中国烟草总公司郑州烟草研究院 | A method of nicotine is purified using subcritical abstraction-molecular clock GC-MS |
| CN108077996A (en) * | 2017-12-06 | 2018-05-29 | 湖北中烟工业有限责任公司 | One preparation method and application for growing tobacco cationic hemicellulose |
| CN108077996B (en) * | 2017-12-06 | 2020-07-24 | 湖北中烟工业有限责任公司 | Preparation method and application of tobacco cationic hemicellulose |
| CN108464192A (en) * | 2018-06-19 | 2018-08-31 | 贵州省贵福菌业发展有限公司 | A kind of oil tea mushroom strains activation medium |
| CN111455705A (en) * | 2020-05-25 | 2020-07-28 | 贺先佑 | Method for manufacturing corrugated paper pulp by using moldy tobacco leaves and other tobacco wastes |
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Application publication date: 20121017 |