CN102733219A - Method for extracting cellulose from tobacco waste based on reductant-oxidant - Google Patents
Method for extracting cellulose from tobacco waste based on reductant-oxidant Download PDFInfo
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- CN102733219A CN102733219A CN2012100425587A CN201210042558A CN102733219A CN 102733219 A CN102733219 A CN 102733219A CN 2012100425587 A CN2012100425587 A CN 2012100425587A CN 201210042558 A CN201210042558 A CN 201210042558A CN 102733219 A CN102733219 A CN 102733219A
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- cellulose
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- tobacco
- tobacco waste
- liquid
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 45
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 45
- 229920002678 cellulose Polymers 0.000 title claims abstract description 32
- 239000001913 cellulose Substances 0.000 title claims abstract description 32
- 239000002699 waste material Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000007800 oxidant agent Substances 0.000 title claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000000967 suction filtration Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000002265 redox agent Substances 0.000 claims description 2
- 230000003381 solubilizing effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 4
- 230000004913 activation Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002154 agricultural waste Substances 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 229960002163 hydrogen peroxide Drugs 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229920002488 Hemicellulose Polymers 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 235000019504 cigarettes Nutrition 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 235000021190 leftovers Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- HQFCOGRKGVGYBB-UHFFFAOYSA-N ethanol;nitric acid Chemical compound CCO.O[N+]([O-])=O HQFCOGRKGVGYBB-UHFFFAOYSA-N 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a chemical extraction method of agricultural waste, particularly a method for extracting cellulose from tobacco waste based on a reductant-oxidant, comprising the following steps: crushing the dried tobacco waste, putting the crushed waste in water to immerse for no less than 6 h to obtain a pretreatment liquid; carrying out solid-liquid separation on the pretreatment liquid and taking the solids, adding a reductant-oxidant solution having the volume of 3-150 times of the volume of the tobacco waste and having the volume percentage of no less than 3%, reacting for at least 15min at 20-90 DEG C to obtain a reaction solution, carrying out solid-liquid separation on the reaction solution, and taking the filter residues, wherein the filter residues are cellulose. The method has the advantages of simple process, energy saving and environmental protection. Compared with the methods for processing tobacco cellulose by traditional acid, alkali activation treatment and other physicochemical treatment, the production cost can be greatly reduced.
Description
Technical field
The present invention relates to the chemical extraction field, particularly the chemical extraction method of agricultural residue.
Background technology
The tobacco planting area of China occupies first place in the world, and tobacco planting and product are processed in the national economy in occupation of important function.The tobacco planting industry has mainly utilized sound tobacco to be used to make cigarette products at present.In the plantation and acquisition process of tobacco, there is every year the tobacco leaf that probably accounts for national tobacco total output 13% to be processed as refuse, become a difficult problem that influences the tobacco business development.Cellulose is a most valuable human natural reproducible resource, is widely used in industries such as weaving, medicine, fermentation producing and ethanol, lactic acid, has very high social value.Utilize agricultural wastes to extract cellulose, become domestic and international biorefinery Study on Technology focus, effectively utilize the cellulose in the tobacco, meet the strategy of sustainable development.Traditional soda acid facture, energy consumption is high, pollutes greatly, and the corrosion equipment does not meet the requirement of energy-saving and emission-reduction.This method is a kind of can the cellulose in the tobacco waste being extracted, and realizes low cost, the low pollution; Low energy consumption; The eco-friendly processing procedure of high efficiency green high-efficient has responded the call of country about energy-saving and emission-reduction, also can bring economic benefit for enterprise simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of method of from tobacco, extracting high purity cellulose, this method operation energy consumption is low, pollutes little, the efficient height, cost is low.
For realizing above-mentioned purpose, technical scheme of the present invention is:
Method based on the tobacco waste cellulose of reductant-oxidant extracts specifically may further comprise the steps:
The A preliminary treatment
Tobacco waste after the oven dry is pulverized, put into the water immersion and be no less than 6 hours, get pretreatment fluid;
The B oxidation reaction
Pretreatment fluid is carried out Separation of Solid and Liquid; Get solid, add and to be equivalent to tobacco waste volume 3-150 percentage by volume doubly and to be not less than 3% redox agent solution, under 20-90 ℃ of condition, carried out sufficient solubilizing reaction at least 15 minutes; Get reactant liquor; Said reactant liquor is carried out Separation of Solid and Liquid, get solid, said solid is a coarse product of cellulose.
Further, after step B, also comprise step C, be specially: in the flushing of gained coarse product of cellulose water, suction filtration, the oven dry of gained solid obtains cellulose.
Further, in the steps A, the particle diameter of said tobacco waste is for being not more than 10 orders.
Further, in step B, the mode of said Separation of Solid and Liquid is a vacuum filtration, and the time of suction filtration is no less than 5 minutes.
Further, in step C, the mode of said Separation of Solid and Liquid is a vacuum filtration, and the time of suction filtration is no less than 5 minutes.
Further, in step C, said filter residue is washed with distilled water, and carry out vacuumize, get cellulose, said baking temperature is 50-80 ℃, and be 10-14 hour drying time.
Beneficial effect of the present invention is: the technology that (1) the present invention adopts is simple, energy-conserving and environment-protective; Handle tobacco material through the reductant-oxidant method and can reach the removal hemicellulose; Lignin; Solable matter can make cellulosic degree of crystallinity become big again, makes cellulose form more regular crystal structure; (2) environmental pollution of the present invention is little, cost is lower, has enlarged the scope of utilizing of crops tobacco wastes greatly, has vast market prospect and huge commercial production potentiality.
The present invention compares following characteristics and progress with traditional handicraft: (1) is handled the plain method of baccy fiber with traditional acid, alkali activation processing and other physical chemistry and is compared; Have the effect that energy consumption is low, pollution is little, efficient is high, can reduce production costs significantly; (2) the ultrasonic activation technology is because ultrasonic technique is easy to generate cavity effect; And be easy to generate the dead angle of production; The bad border of waste liquor contamination that the soda acid facture produces, and corrosion equipment, the NaOH cost is higher; These factors have all restricted the suitability for industrialized production of cellulosic extraction in the plant waste, and the reductant-oxidant method preferably resolves above problem.
Description of drawings
Fig. 1 is the plain SEM figure of baccy fiber of the tobacco material of untreated (be untreated and refer to that this figure is the exterior view of raw material own);
Fig. 2 is the plain SEM figure of the baccy fiber after time reductant-oxidant is handled.
The specific 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 leftover bits and pieces, tobacco waste is a large amount of byproducts that produce in the production of cigarettes, is rich in various organic principles 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 Co., Ltd, and its moisture accounts for 7% of tobacco waste gross mass.
Among the following embodiment, cellulosic purity is meant cellulosic yield.
Cellulosic method for detecting purity is the nitric acid Ethanol Method.Lignin, the detection method of hemicellulose purity are the normal form fibre method.Among the following embodiment in the tobacco waste cellulosic total content be 34%.
Embodiment 1
Getting the 100g particle diameter is 20 purpose tobacco wastes, boiling 1 hour time, Separation of Solid and Liquid then in the water; Get solid, the concentration expressed in percentage by volume that adds 20 times of volumes being equivalent to said solid is 60% ethanol, under 100 ℃ of conditions, stirs 2 hours; Said reactant liquor is filtered; The gained filter residue moves into baking oven, dries to constant mass in 105 ℃ to be 39.1g, and content of cellulose is 34% in the filter residue.
Embodiment 2
The NaOH that accurately takes by weighing 170g is dissolved in the distilled water of 510mL, is configured to mass percentage concentration and is 25% NaOH solution.Taking by weighing the 100g particle diameter is that 20 purpose tobacco wastes are put into three-necked bottle; Add the 500mL mass percentage concentration again and be 25% NaOH solution, mechanical agitation reaction 1 hour, reaction finish the back and use the distilled water wash suction filtration; Till being neutrality to suction filtration liquid; The gained filter residue moves into baking oven, dries to the constant mass drying in 105 ℃ to be 49.1g, and content of cellulose only accounts for 65% of cellulose gross mass in the filter residue.
Embodiment 3
Taking by weighing the 100g particle diameter is that 20 purpose tobacco wastes are put into three-necked bottle; Add the 500mL mass concentration again and be 10% hydrochloric acid solution, mechanical agitation reaction 1.5 hours, reaction finish the back and use the distilled water wash suction filtration; Till being neutrality to suction filtration liquid; The gained filter residue moves into baking oven, dries to the constant mass drying in 105 ℃ to be 48.7g, and content of cellulose only accounts for 67% of cellulose gross mass in the filter residue.
Embodiment 4
Taking by weighing the 100g particle diameter is that 20 purpose tobacco wastes are put into three-necked bottle, adds the 500mL aqueous solution again, and ultrasonic power is 350w ultrasonic reaction 1.5 hours, and reaction finishes the back and uses the distilled water wash suction filtration, be neutrality to suction filtration liquid till.The gained solid is put into the 1 hour time of boiling water boiling, after the Separation of Solid and Liquid, get solid; The concentration expressed in percentage by volume that adds 20 times of volumes being equivalent to tobacco is 60% ethanol; Under 100 ℃ of conditions, stir 2 hour time, said reactant liquor is carried out Separation of Solid and Liquid, the gained filter residue moves into baking oven; Drying to the constant mass drying in 105 ℃ is 47.7g, and content of cellulose only accounts for 70% of cellulose gross mass in the filter residue.
Embodiment 5
Getting the 100g particle diameter is 20 purpose tobacco wastes, and its SEM figure is as shown in Figure 1.Put it into hydrogenperoxide steam generator, solid-to-liquid ratio 1: 10, the reaction time is more than 60 minutes; 30 ℃ of reaction temperatures; The concentration expressed in percentage by volume of hydrogenperoxide steam generator is 10%, filters after having reacted, and the gained filter residue moves into baking oven; Drying to constant mass in 105 ℃ is 38.3g, and content of cellulose only accounts for 81% of cellulose gross mass in the filter residue.Filter residue is as shown in Figure 2, compares with Fig. 1, and it is loose that the tobacco compact texture is destroyed, becomes.In addition, selecting volume fraction for use is the frerrous chloride of 3-10%, nitrous acid, and sulfurous acid, hypochlorous acid, other reductant-oxidant of sodium thiosulfate are handled filter residue respectively, and before the processing, the raw material surface texture is level and smooth, and is in order fine and close.After treatment, material is owing to removed more hemicellulose and its structural deterioration of lignin is obvious, and a large amount of folds appear in the surface, hole, and it is fluffy, at random that structure becomes, and specific area increases.
Embodiment 6
Getting the 100g particle diameter is 20 purpose tobacco wastes, puts into hydrogenperoxide steam generator, solid-to-liquid ratio 1: 15; In 60 minutes reaction time, 70 ℃ of reaction temperatures, the volume fraction of hydrogenperoxide steam generator are 8%; Filter after having reacted; The gained filter residue moves into baking oven, dries to constant mass in 105 ℃ to be 37.7g, and content of cellulose only accounts for 83% of cellulose gross mass in the filter residue.
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 (6)
1. the method for extracting based on the tobacco waste cellulose of reductant-oxidant is characterized in that, specifically may further comprise the steps:
The A preliminary treatment
Tobacco waste is pulverized, put into the water immersion and be no less than 6 hours, get pretreatment fluid;
The B oxidation reaction
Pretreatment fluid is carried out Separation of Solid and Liquid; Get solid, add and to be equivalent to tobacco waste volume 3-150 percentage by volume doubly and to be not less than 3% redox agent solution, under 20-90 ℃ of condition, carried out sufficient solubilizing reaction at least 15 minutes; Get reactant liquor; Said reactant liquor is carried out Separation of Solid and Liquid, get solid, said solid is a coarse product of cellulose.
2. method according to claim 1 is characterized in that, after step B, also comprises step C, is specially: in the flushing of gained coarse product of cellulose water, and suction filtration, the oven dry of gained solid obtains cellulose.
3. method according to claim 1 is characterized in that, in the steps A, the particle diameter of said tobacco waste is not more than 10 orders.
4. according to the said method of claim 1, it is characterized in that in step B, the mode of said Separation of Solid and Liquid is a vacuum filtration, the time of suction filtration is no less than 5 minutes.
5. according to the said method of claim 1, it is characterized in that in step C, the mode of said Separation of Solid and Liquid is a vacuum filtration, the time of suction filtration is no less than 5 minutes.
6. method according to claim 1 is characterized in that, in step C, said filter residue is washed with distilled water, and carries out vacuumize, gets cellulose, and said baking temperature is 50-80 ℃, and be 10-14 hour drying time.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210042558.7A CN102733219B (en) | 2012-02-23 | 2012-02-23 | Method for extracting cellulose from tobacco waste based on reductant-oxidant |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210042558.7A CN102733219B (en) | 2012-02-23 | 2012-02-23 | Method for extracting cellulose from tobacco waste based on reductant-oxidant |
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| CN102733219A true CN102733219A (en) | 2012-10-17 |
| CN102733219B CN102733219B (en) | 2015-04-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103643577A (en) * | 2013-11-27 | 2014-03-19 | 上海大学 | Method for preparation of nano-cellulose whiskers from garlic skins |
| CN105189858A (en) * | 2013-03-21 | 2015-12-23 | 日本烟草产业株式会社 | Production method for black liquor and production method for liquid containing flavoring component |
| 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 |
| WO2021001557A1 (en) | 2019-07-03 | 2021-01-07 | Futamura Chemical Uk Ltd | Extraction method |
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| WO2000047701A2 (en) * | 1999-02-10 | 2000-08-17 | Eastman Chemical Company | Corn fiber for the production of advanced chemicals and materials |
| CN1779070A (en) * | 2005-08-09 | 2006-05-31 | 华南理工大学 | Full component separation for cell wall of agricultural refuse |
| CN101158126A (en) * | 2007-10-27 | 2008-04-09 | 广西大学 | Pulping method for plant fibre raw material combined with biology |
| CN101864455A (en) * | 2010-04-11 | 2010-10-20 | 中国海洋大学 | A kind of oxidative degradation pretreatment enteromorpha as raw material that utilizes carries out the method that alcohol fuel transforms |
-
2012
- 2012-02-23 CN CN201210042558.7A patent/CN102733219B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000047701A2 (en) * | 1999-02-10 | 2000-08-17 | Eastman Chemical Company | Corn fiber for the production of advanced chemicals and materials |
| CN1779070A (en) * | 2005-08-09 | 2006-05-31 | 华南理工大学 | Full component separation for cell wall of agricultural refuse |
| CN101158126A (en) * | 2007-10-27 | 2008-04-09 | 广西大学 | Pulping method for plant fibre raw material combined with biology |
| CN101864455A (en) * | 2010-04-11 | 2010-10-20 | 中国海洋大学 | A kind of oxidative degradation pretreatment enteromorpha as raw material that utilizes carries out the method that alcohol fuel transforms |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105189858A (en) * | 2013-03-21 | 2015-12-23 | 日本烟草产业株式会社 | Production method for black liquor and production method for liquid containing flavoring component |
| US10851494B2 (en) | 2013-03-21 | 2020-12-01 | Japan Tobacco Inc. | Method for preparing black liquor and method for preparing flavor component-containing liquid |
| CN103643577A (en) * | 2013-11-27 | 2014-03-19 | 上海大学 | Method for preparation of nano-cellulose whiskers from garlic skins |
| CN103643577B (en) * | 2013-11-27 | 2015-10-28 | 上海大学 | A kind of method utilizing garlic skin to prepare nano-cellulose whisker |
| 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 |
| WO2021001557A1 (en) | 2019-07-03 | 2021-01-07 | Futamura Chemical Uk Ltd | Extraction method |
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