CN102733217B - Method for extracting cellulose from tobacco waste based on water-alcohol oxidation process - Google Patents
Method for extracting cellulose from tobacco waste based on water-alcohol oxidation process Download PDFInfo
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- CN102733217B CN102733217B CN201210042566.1A CN201210042566A CN102733217B CN 102733217 B CN102733217 B CN 102733217B CN 201210042566 A CN201210042566 A CN 201210042566A CN 102733217 B CN102733217 B CN 102733217B
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- tobacco waste
- filter residue
- cellulose
- solid
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- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 53
- 241000208125 Nicotiana Species 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000002699 waste material Substances 0.000 title claims abstract description 38
- 229920002678 cellulose Polymers 0.000 title claims abstract description 26
- 239000001913 cellulose Substances 0.000 title claims abstract description 24
- 230000003647 oxidation Effects 0.000 title claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000007800 oxidant agent Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 30
- 239000007787 solid Substances 0.000 claims description 18
- 229960002163 hydrogen peroxide Drugs 0.000 claims description 15
- 238000009835 boiling Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000003828 vacuum filtration Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 230000003381 solubilizing effect Effects 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 3
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 3
- 239000002265 redox agent Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 6
- 229920002488 Hemicellulose Polymers 0.000 abstract description 5
- 229920005610 lignin Polymers 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000002154 agricultural waste Substances 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 235000010980 cellulose Nutrition 0.000 description 16
- 239000000835 fiber Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 235000019504 cigarettes Nutrition 0.000 description 3
- 235000021190 leftovers Nutrition 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 239000006227 byproduct 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
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- HQFCOGRKGVGYBB-UHFFFAOYSA-N ethanol;nitric acid Chemical group CCO.O[N+]([O-])=O HQFCOGRKGVGYBB-UHFFFAOYSA-N 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- 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 water-alcohol oxidation process, comprising the following steps: crushing the tobacco waste, putting the crushed waste in water to boil for no less than 20 min and dewatering to obtain a pretreatment material; adding an alcoholic solution having the volume of 5-70 times of the volume of the tobacco waste in the obtained pretreatment material, reacting for at least 30min at 80-100 DEG C, and carrying out solid-liquid separation to obtain filter residues, wherein the volume percentage of the alcoholic solution is 20-90 %, and the filter residues are crude cellulose. The method has the advantages of simple process, energy saving and environmental protection, and the purposes of removing residual lignin, extracting residual hemicellulose and soluble substance can be achieved by using reductant-oxidants to process the tobacco raw material. By using the water-alcohol oxidation process to process tobacco cellulose first and using the reductant-oxidant solution to oxidize and then extracting, the extraction efficiency is raised about by 150% compared with using the water-alcohol oxidation process along, thus the extraction efficiency is greatly raised.
Description
Technical field
The present invention relates to chemical field, particularly the chemical extraction methods of agricultural residue.
Background technology
Energy-saving and emission-reduction and to the comprehensive utilization of renewable resource at present by the whole world is paid close attention to.Cultivated area and the output of China's tobacco plant all occupy first place in the world, and as tobacco leaf production big country, China except production 450 ~ 5,000,000 tons, tobacco leaf, still has the leftover bits and pieces such as the tobacco leaf of nearly 25%, offal to go out of use, can not be used for production of cigarettes every year.Along with the proposition that " 12 " plan, how can better utilize tobacco waste, be current focal point.Cellulose, as a kind of natural macromolecular material, is widely used in the industry such as medicine, papermaking, can also be used to produce PLA, methylcellulose, ethyl cellulose, microcrystalline cellulose etc., and market prospects are huge.Containing a large amount of celluloses in tobacco waste, if well can be utilized these baccy fiber elements, a large amount of pollution problems can not only be solved, huge contribution can also be made for the sound development of national economy.Current pretreatment mode and the solvent of dissolving cellulos, because cost is high, it is large to pollute, efficiency is low, the serious extensive use hindering baccy fiber element.Containing abundant cellulose in tobacco.This method adopts a kind of novel water alcohol oxidizing process the cellulose in tobacco waste can not only to be extracted, and reach low cost, low stain, the requirement of low energy consumption, both the call of country about built environment friendly society had been responded, again for society brings great economic benefit and social benefit.
Summary of the invention
The object of the present invention is to provide and extract cellulosic method from tobacco waste, the method is simple to operate, and yield is high, is applicable to suitability for industrialized production.
For achieving the above object, technical scheme of the present invention is:
From tobacco waste, extract cellulosic method based on water alcohol oxidizing process, specifically comprise the following steps:
A pretreatment of raw material
Tobacco waste is pulverized, puts into water boiling and be no less than 20 minutes, remove moisture content, obtain preliminary treatment material;
B alcohol wash
Add in steps A gained preliminary treatment material and be equivalent to described tobacco waste volume 5-70 alcoholic solution doubly, under 80-100 DEG C of condition, react at least 30 minutes, Separation of Solid and Liquid, obtain filter residue, the volumetric concentration of described alcoholic solution is 20%-90%, and described filter residue is coarse product of cellulose.
Wherein, after stepb, also comprise oxidation step, be specially: gained filter residue adds and is equivalent to the redox agent solution that filter residue volume 5-40 percentage by volume is doubly not less than 2% in stepb, under 20-90 DEG C of condition, carry out sufficient solubilizing reaction at least 20 minutes, obtain reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, gets solid, rinse, dry, obtain high purity cellulose.
Wherein, in steps A, the particle diameter of described tobacco waste is not more than 10 orders.
Wherein, in steps A, pulverized by tobacco waste, put into boiling water boiling 20-120 minute, vacuum filtration removes moisture content, obtains preliminary treatment material.
Wherein, in stepb, the mode of described Separation of Solid and Liquid is vacuum filtration, and the time of suction filtration is no less than 5 minutes.
Wherein, in stepb, described reaction is carried out under stirring.
Wherein, described reductant-oxidant is specially hydrogen peroxide, frerrous chloride, nitrous acid, and any one or more in sulfurous acid, hypochlorous acid, sodium thiosulfate mixes.
Wherein, described reductant-oxidant to be percent by volume be 10% hydrogenperoxide steam generator.
Wherein, washed by described solid water, and carry out vacuumize, obtain cellulose, described baking temperature is 50-80 DEG C, and drying time is 10-14 hour.
Preferred version of the present invention is: in steps A gained preliminary treatment material, add the alcoholic solution being equivalent to described tobacco waste volume 40 times, react 120 minutes under 100 DEG C of conditions, Separation of Solid and Liquid, obtains filter residue, the percent by volume of described alcoholic solution is 70%, and described filter residue is coarse product of cellulose; Described alcoholic solution can be ethanolic solution.
Gained filter residue add the volume fraction being equivalent to tobacco waste volume 26 times be 10% hydrogenperoxide steam generator, sufficient solubilizing reaction is carried out at least 40 minutes under 70 DEG C of conditions, obtain reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, gets solid, described solid water is washed, and carry out vacuumize, obtain cellulose, described baking temperature is 80 DEG C, and drying time is 10 hours.
Hinge structure of the present invention has following advantage: (1) the present invention uses water alcohol method to extract hemicellulose in tobacco, lignin, solable matter, and can reclaim ethanol; (2) technique adopted is simple, energy-conserving and environment-protective, can reach removal residual lignin, also can extract residue hemicellulose, solable matter by reductant-oxidant process tobacco material; (3) environmental pollution of the present invention is little, cost is lower, and cellulose purity is high, and degree of crystallinity is high, and what expand crops tobacco waste greatly utilizes scope, has wide market prospects and huge industrial production potentiality.(4) first adopt water alcohol method process baccy fiber element, then extract with after reductant-oxidant solution oxide, with independent water alcohol method, its extraction efficiency improves 150% nearly, drastically increases extraction efficiency.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the baccy fiber element of the tobacco material of untreated (this figure of untreated finger is the exterior view of raw material own);
Fig. 2 is the SEM figure of the baccy fiber element after the process of water alcohol;
Fig. 3 is the SEM figure of baccy fiber element after water alcohol oxidation processes.
Detailed description of the invention
In the present invention, the tobacco waste of indication, has another name called tobacco leftovers, is specially: tobacco leaf, the offal of useless time.Low, hypo-tobacco leaf and cigarette leftover bits and pieces in a large number, tobacco waste is a large amount of byproducts produced in production of cigarettes, is rich in various organic principle and secondary metabolite.Tobacco waste also can make material substitution with tobacco.
Tobacco waste in following embodiment comes from Chongqing Yin Fu biological organic fertilizer Co., Ltd, and its moisture accounts for 7% of tobacco waste gross mass.
In following embodiment, cellulosic purity refers to cellulosic yield.
Cellulosic method for detecting purity is nitric acid Ethanol Method.Lignin, the detection method of hemicellulose purity is normal form fibre method.
Embodiment 1
Tobacco waste after being dried by 100g is pulverized as particle diameter is 20 orders, puts into boiling water boiling 20 minutes, and vacuum filtration removes moisture content, obtains preliminary treatment material; The ethanolic solution being equivalent to described preliminary treatment material volume 15 times is added in gained preliminary treatment material, the percentage by volume of described ethanolic solution is 70%, at least 120 minutes are reacted under 100 DEG C of conditions, vacuum filtration removes moisture content, obtain filter residue, gained filter residue moves into baking oven, and be 19.7g in 105 DEG C of oven dry to constant mass, in filter residue, content of cellulose is 50.7%.
Embodiment 2
Without the tobacco waste of any process, its SEM schemes as shown in Figure 1, tobacco smooth surface, neat, connects closely.
Tobacco waste after being dried by 100g is pulverized as particle diameter is 20 orders, puts into boiling water boiling 60 minutes, and vacuum filtration removes moisture content, obtains preliminary treatment material; The ethanolic solution being equivalent to described tobacco waste volume 15 times is added in gained preliminary treatment material, the percentage by volume of described ethanolic solution is 70%, at least 120 minutes are reacted under 100 DEG C of conditions, vacuum filtration removes moisture content, obtain filter residue, described filter residue is coarse product of cellulose, there is the fracture of key as shown in Figure 2 in tobacco, have depression, hole occur.
Hydrogenperoxide steam generator is put in described filter residue, the solid-liquid volume ratio 1: 10 of filter residue and hydrogenperoxide steam generator, 60 minutes reaction time, reaction temperature 30 DEG C, hydrogenperoxide steam generator concentration 10%, filters after having reacted, gained filter residue, its SEM schemes as shown in Figure 3, and that compares with Fig. 2, tobacco compact texture is destroyed, becomes is loose.Separately, select percentage by volume to be the frerrous chloride of 2-10%, nitrous acid, other reductant-oxidant of sulfurous acid, hypochlorous acid, sodium thiosulfate processes filter residue respectively, and before process, raw material surface texture is level and smooth, dense regular.After treatment, material is obvious owing to eliminating more hemicellulose and its structural deterioration of lignin, and a large amount of fold appears in surface, hole, and it is fluffy, at random that structure becomes, and specific area increases.
Embodiment 3
Tobacco waste after being dried by 100g is pulverized as particle diameter is 20 orders, puts into boiling water boiling 60 minutes, and vacuum filtration removes moisture content, obtains preliminary treatment material; The ethanolic solution being equivalent to described tobacco waste volume 20 times is added in gained preliminary treatment material, the percentage by volume of described ethanolic solution is 70%, under 100 DEG C of conditions, react at least 120 minutes, and vacuum filtration removes moisture content, obtain filter residue, described filter residue is coarse product of cellulose.
Hydrogenperoxide steam generator is put in described filter residue, the solid-liquid volume ratio 1: 5 of filter residue and hydrogenperoxide steam generator, 60 minutes reaction time, reaction temperature 30 DEG C, the concentration expressed in percentage by volume 8% of hydrogenperoxide steam generator, filters after having reacted, gained filter residue, move into baking oven, dry 20.8g to constant mass in 105 DEG C, filter residue content of cellulose is 63.0%.
Embodiment 4
Tobacco waste after being dried by 100g is pulverized as particle diameter is 20 orders, puts into boiling water boiling 60 minutes, and vacuum filtration removes moisture content, obtains preliminary treatment material; The ethanolic solution being equivalent to described tobacco waste volume 40 times is added in gained preliminary treatment material, the volume mass concentration of described ethanolic solution is 70%, under 100 DEG C of conditions, react at least 120 minutes, and vacuum filtration removes moisture content, obtain filter residue, described filter residue is coarse product of cellulose.
Hydrogenperoxide steam generator is put in described filter residue, the solid-liquid volume ratio 1: 26 of filter residue and hydrogenperoxide steam generator, 60 minutes reaction time, reaction temperature 30 DEG C, hydrogenperoxide steam generator concentration 8%, filters after having reacted, gained filter residue, move into baking oven, dry 21.5g to constant mass in 105 DEG C, filter residue content of cellulose is 65.2%.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (8)
1. from tobacco waste, extract cellulosic method based on water alcohol oxidizing process, it is characterized in that, specifically
Comprise the following steps:
A pretreatment of raw material
Tobacco waste is pulverized, puts into water boiling and be no less than 20 minutes, remove moisture content, obtain preliminary treatment material;
B alcohol wash
Add in steps A gained preliminary treatment material and be equivalent to described tobacco waste volume 5-70 alcoholic solution doubly, under 80-100 DEG C of condition, react at least 30 minutes, Separation of Solid and Liquid, obtain filter residue, the volumetric concentration of described alcoholic solution is 20%-90%, and described filter residue is coarse product of cellulose;
C oxidation step
Gained filter residue adds and is equivalent to the redox agent solution that filter residue volume 5-40 percentage by volume is doubly not less than 2% in stepb, sufficient solubilizing reaction is carried out at least 20 minutes under 20-90 DEG C of condition, obtain reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, get solid, rinse, dries, obtains high purity cellulose; Described reductant-oxidant is specially hydrogen peroxide, frerrous chloride, nitrous acid, and any one or more in sulfurous acid, hypochlorous acid, sodium thiosulfate mixes.
2. method according to claim 1, is characterized in that, in steps A, the particle diameter of described tobacco waste is not more than 10 orders.
3. method according to claim 1, is characterized in that, in steps A, pulverized by tobacco waste, put into boiling water boiling 20-120 minute, vacuum filtration removes moisture content, obtains preliminary treatment material.
4. method according to claim 1, is characterized in that, in stepb, the mode of described Separation of Solid and Liquid is vacuum filtration, and the time of suction filtration is no less than 5 minutes.
5. method according to claim 1, is characterized in that, in stepb, described reaction is carried out under stirring.
6. method according to claim 1, is characterized in that, described reductant-oxidant to be percentage by volume be 10% hydrogenperoxide steam generator.
7. method according to claim 1, is characterized in that, oxidation step, is washed by described solid water, and carries out vacuumize, obtain cellulose, and described baking temperature is 50-80 DEG C, and drying time is 10-14 hour.
8. method according to claim 1, it is characterized in that, the alcoholic solution being equivalent to described tobacco waste volume 40 times is added in steps A gained preliminary treatment material, at least 120 minutes are reacted under 100 DEG C of conditions, Separation of Solid and Liquid, obtain filter residue, the percent by volume of described alcoholic solution is 70%, and described filter residue is coarse product of cellulose;
Gained filter residue add the percentage by volume being equivalent to tobacco waste volume 26 times be 10% hydrogenperoxide steam generator, sufficient solubilizing reaction is carried out 40 minutes under 70 DEG C of conditions, obtain reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, gets solid, described solid water is washed, and carry out vacuumize, obtain cellulose, described baking temperature is 80 DEG C, and drying time is 10 hours.
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| CN201210042566.1A CN102733217B (en) | 2012-02-23 | 2012-02-23 | Method for extracting cellulose from tobacco waste based on water-alcohol oxidation process |
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| CN109306362A (en) * | 2017-07-27 | 2019-02-05 | 重庆恒远晋通科技有限公司 | A method of based on water alcohol oxidizing process preparing ethyl alcohol from sweet sorghum |
| CN111945453A (en) * | 2020-08-18 | 2020-11-17 | 何建设 | Preparation method of loofah sponge dissolving pulp |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10151952A1 (en) * | 2001-10-22 | 2003-04-30 | Duempert Hellmuth | Organic solvent-free recovery of materials e.g. cellulosics or lignin from a plant biomass in an 'Aquasolf' process involves use of water under sub-critical conditions as the decomposing and extracting solvent |
| CN101143881A (en) * | 2007-10-11 | 2008-03-19 | 孔延华 | Method for synchronously extracting hemicellulose, cellulose and lignin and reclaiming phenolic acid compounds |
| CN101235604A (en) * | 2007-01-31 | 2008-08-06 | 中国科学院化学研究所 | Method for extracting cellulose from straw |
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| US20070249825A1 (en) * | 2006-04-21 | 2007-10-25 | Sau Arjun C | Decolorized raw cotton linters and preparation of ether derivatives therefrom |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10151952A1 (en) * | 2001-10-22 | 2003-04-30 | Duempert Hellmuth | Organic solvent-free recovery of materials e.g. cellulosics or lignin from a plant biomass in an 'Aquasolf' process involves use of water under sub-critical conditions as the decomposing and extracting solvent |
| CN101235604A (en) * | 2007-01-31 | 2008-08-06 | 中国科学院化学研究所 | Method for extracting cellulose from straw |
| CN101143881A (en) * | 2007-10-11 | 2008-03-19 | 孔延华 | Method for synchronously extracting hemicellulose, cellulose and lignin and reclaiming phenolic acid compounds |
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