CN102733219B - 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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- CN102733219B CN102733219B CN201210042558.7A CN201210042558A CN102733219B CN 102733219 B CN102733219 B CN 102733219B CN 201210042558 A CN201210042558 A CN 201210042558A CN 102733219 B CN102733219 B CN 102733219B
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- cellulose
- solid
- tobacco
- tobacco waste
- suction filtration
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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
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000002699 waste material Substances 0.000 title claims abstract description 29
- 239000007800 oxidant agent Substances 0.000 title claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 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
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000000967 suction filtration Methods 0.000 claims description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 229960002163 hydrogen peroxide Drugs 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000003381 solubilizing effect Effects 0.000 claims description 2
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000004913 activation Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 239000002154 agricultural waste 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000047 product Substances 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
- 238000005516 engineering process Methods 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
- 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
- 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 group CCO.O[N+]([O-])=O HQFCOGRKGVGYBB-UHFFFAOYSA-N 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
- 238000009776 industrial production Methods 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
- 239000002265 redox agent Substances 0.000 description 1
- 229930000044 secondary metabolite Natural products 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
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 chemical extraction field, particularly the chemical extraction methods of agricultural residue.
Background technology
The tobacco planting area of China occupies first place in the world, tobacco planting and Product processing in national economy in occupation of important function.Tobacco planting industry mainly make use of sound tobacco at present for making cigarette products.In the plantation and acquisition process of tobacco, there is the tobacco leaf probably accounting for national tobacco total output 13% to be processed as refuse every year, become the difficult problem affecting tobacco business development.Cellulose is the most valuable natural reproducible resources of the mankind, is widely used in weaving, medicine, industry such as fermentation producing and ethanol, lactic acid etc., has very high social value.Utilize agricultural wastes to extract cellulose, become the study hotspot of domestic and international biorefinery technology, effectively utilized the cellulose in tobacco, meet the strategy of sustainable development.Traditional acid-alkali treatment method, energy consumption is high, pollutes large, and corrosion equipment, does not meet the requirement of energy-saving and emission-reduction.This method is a kind of cellulose in tobacco waste can being extracted, and realizes low cost, low stain, 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 extracting high purity cellulose from tobacco, the method operation energy consumption is low, and pollute little, efficiency is high, and cost is low.
For achieving the above object, technical scheme of the present invention is:
Based on the method that the tobacco waste cellulose of reductant-oxidant extracts, specifically comprise the following steps:
A preliminary treatment
Tobacco waste after drying is pulverized, puts into water immersion and be no less than 6 hours, obtain pretreatment fluid;
B oxidation reaction
Pretreatment fluid is carried out Separation of Solid and Liquid, get solid, add and be equivalent to the redox agent solution that tobacco waste volume 3-150 percentage by volume is doubly not less than 3%, sufficient solubilizing reaction is carried out at least 15 minutes under 20-90 DEG C of condition, obtain reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, gets solid, described solid is coarse product of cellulose.
Further, after stepb, also comprise step C, be specially: rinse at gained coarse product of cellulose water, suction filtration, gained solid is dried, and obtains cellulose.
Further, in steps A, the particle diameter of described tobacco waste is for being not more than 10 orders.
Further, 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.
Further, in step C, the mode of described Separation of Solid and Liquid is vacuum filtration, and the time of suction filtration is no less than 5 minutes.
Further, in step C, washed by described filter residue distilled water, and carry out vacuumize, obtain cellulose, described baking temperature is 50-80 DEG C, and drying time is 10-14 hour.
Beneficial effect of the present invention is: the technique that (1) the present invention adopts is simple, energy-conserving and environment-protective, removal hemicellulose can be reached by reductant-oxidant method process tobacco material, lignin, solable matter, cellulosic degree of crystallinity can be made again to become large, make cellulose form more regular crystal structure; (2) environmental pollution of the present invention is little, cost is lower, and what expand crops tobacco waste greatly utilizes scope, has wide market prospects and huge industrial production potentiality.
The present invention has following characteristics and progress compared with traditional handicraft: compared with the method for (1) and traditional acid, alkali activation processing and other physical chemistry process baccy fiber element, have energy consumption low, pollute little, that efficiency is high effect, production cost can be reduced significantly; (2) ultrasonic activation technology easily produces cavity effect due to ultrasonic technique, and easily produce the dead angle produced, the waste liquor contamination bad border that acid-alkali treatment method produces, and corrosion equipment, NaOH cost is higher, these factors all constrain the suitability for industrialized production of cellulosic extraction in plant waste, and reductant-oxidant method preferably resolves above problem.
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 time reductant-oxidant process.
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.In following embodiment, in tobacco waste, cellulosic total content is 34%.
Embodiment 1
Getting 100g particle diameter is 20 object tobacco wastes, boiling 1 hours in water, then Separation of Solid and Liquid, get solid, the concentration expressed in percentage by volume adding the volume 20 times being equivalent to described solid is the ethanol of 60%, carries out stirring 2 hours under 100 DEG C of conditions, described reactant liquor is filtered, gained filter residue moves into baking oven, and be 39.1g in 105 DEG C of oven dry to constant mass, in filter residue, content of cellulose is 34%.
Embodiment 2
The NaOH accurately taking 170g is dissolved in the distilled water of 510mL, is configured to the NaOH solution that mass percentage concentration is 25%.Taking 100g particle diameter is that 20 object tobacco wastes put into three-necked bottle, add the NaOH solution that 500mL mass percentage concentration is 25% again, mechanic whirl-nett reaction 1 hour, reaction terminates rear distilled water and washs suction filtration, to suction filtration liquid is neutrality, gained filter residue moves into baking oven, and drying to constant mass drying in 105 DEG C is 49.1g afterwards, and in filter residue, content of cellulose only accounts for 65% of cellulose gross mass.
Embodiment 3
Taking 100g particle diameter is that 20 object tobacco wastes put into three-necked bottle, add the hydrochloric acid solution that 500mL mass concentration is 10% again, mechanic whirl-nett reaction 1.5 hours, reaction terminates rear distilled water and washs suction filtration, to suction filtration liquid is neutrality, gained filter residue moves into baking oven, and drying to constant mass drying in 105 DEG C is 48.7g afterwards, and in filter residue, content of cellulose only accounts for 67% of cellulose gross mass.
Embodiment 4
Taking 100g particle diameter is that 20 object tobacco wastes put into three-necked bottle, then adds the 500mL aqueous solution, and ultrasonic power is 350w ultrasonic reaction 1.5 hours, and reaction terminates rear distilled water and washs suction filtration, to suction filtration liquid is neutrality.Gained solid is put into boiling water boiling 1 hours, after Separation of Solid and Liquid, get solid, the concentration expressed in percentage by volume adding the volume 20 times being equivalent to tobacco is the ethanol of 60%, under 100 DEG C of conditions, carry out stirring 2 hours, described reactant liquor is carried out Separation of Solid and Liquid, gained filter residue moves into baking oven, drying to constant mass drying in 105 DEG C is 47.7g afterwards, and in filter residue, content of cellulose only accounts for 70% of cellulose gross mass.
Embodiment 5
Getting 100g particle diameter is 20 object tobacco wastes, and its SEM schemes as shown in Figure 1.Put it into hydrogenperoxide steam generator, solid-to-liquid ratio 1: 10, more than 60 minutes reaction time, reaction temperature 30 DEG C, the concentration expressed in percentage by volume of hydrogenperoxide steam generator is 10%, filters after having reacted, and gained filter residue moves into baking oven, be 38.3g in 105 DEG C of oven dry to constant mass, in filter residue, content of cellulose only accounts for 81% of cellulose gross mass.Filter residue as shown in Figure 2, is compared with Fig. 1, tobacco compact texture is destroyed, become loose.Separately, select volume fraction to be the frerrous chloride of 3-10%, 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 6
Getting 100g particle diameter is 20 object tobacco wastes, put into hydrogenperoxide steam generator, solid-to-liquid ratio 1: 15,60 minutes reaction time, reaction temperature 70 DEG C, the volume fraction of hydrogenperoxide steam generator is 8%, filter after having reacted, gained filter residue moves into baking oven, and be 37.7g in 105 DEG C of oven dry to constant mass, in filter residue, content of cellulose only accounts for 83% of cellulose gross mass.
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 (4)
1., based on the method that the tobacco waste cellulose of reductant-oxidant extracts, it is characterized in that, specifically comprise the following steps:
A preliminary treatment
Tobacco waste is pulverized, puts into water immersion and be no less than 6 hours, obtain pretreatment fluid;
B oxidation reaction
Pretreatment fluid is carried out Separation of Solid and Liquid, get solid, add the hydrogenperoxide steam generator being equivalent to tobacco waste volume 3-150 percentage by volume 8% or 10% doubly, sufficient solubilizing reaction is carried out at least 15 minutes under 20-90 DEG C of condition, obtain reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, gets solid, described solid is coarse product of cellulose;
After stepb, also comprise step C, be specially: rinsed by gained coarse product of cellulose water, suction filtration, gained solid is dried, and obtains cellulose; In step C, the filter residue distilled water obtained by described suction filtration washs, and carries out vacuumize, obtains cellulose, and described baking temperature is 50-80 DEG C, and drying time is 10-14 hour.
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, it 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.
4. method according to claim 1, it is characterized in that, in step C, the mode of described suction filtration is vacuum filtration, and the time of suction filtration is no less than 5 minutes.
Priority Applications (1)
| 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 CN102733219A (en) | 2012-10-17 |
| CN102733219B true CN102733219B (en) | 2015-04-01 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2977511B1 (en) * | 2013-03-21 | 2020-02-12 | Japan Tobacco Inc. | Production method for black liquor and production method for liquid containing flavoring component |
| CN103643577B (en) * | 2013-11-27 | 2015-10-28 | 上海大学 | A kind of method utilizing garlic skin to prepare nano-cellulose whisker |
| 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 |
| EP3994181A1 (en) | 2019-07-03 | 2022-05-11 | Futamura Chemical UK Limited | Extraction method |
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 |
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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 |
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| CN102733219A (en) | 2012-10-17 |
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