CN102304865B - Method for extracting cellulose from tobacco - Google Patents
Method for extracting cellulose from tobacco Download PDFInfo
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- CN102304865B CN102304865B CN 201110248519 CN201110248519A CN102304865B CN 102304865 B CN102304865 B CN 102304865B CN 201110248519 CN201110248519 CN 201110248519 CN 201110248519 A CN201110248519 A CN 201110248519A CN 102304865 B CN102304865 B CN 102304865B
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/241—Extraction of specific substances
- A24B15/245—Nitrosamines
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to the field of chemical industry and particularly relates to a process for extracting cellulose from vegetable. The method specifically comprises the following steps of: adding 1-butyl-3-methylimidazolium chloride in an amount which is 10 to 15 times mass of tobacco into tobacco, performing full dissolution reaction at the temperature of between 80 and 110 DEG C to obtain reaction liquor, performing solid-liquid separation on the reaction liquor to obtain liquor, namely a cellulose solution; and adding deionized water in an amount which is 3 to 5 times volume of the cellulose solution, and stirring for more than or equal to 30 minutes and then filtering to obtain filter residues, namely cellulose. Compared with the conventional method for performing activating treatment on tobacco cellulose by using acid and alkali, the process has the advantages that: due to the steam explosion pretreatment, the effects of low consumption, low pollution and high efficiency are achieved, and production cost can be obviously reduced; and compared with a method for dissolving cellulose by using ionic liquid only, the method for activating tobacco cellulose by steam explosion first and then dissolving cellulose by using ionic liquid has the advantage that the dissolving efficiency is improved by about 60 percent.
Description
Technical field
The present invention relates to chemical field, particularly extract cellulosic technique from plant.
Background technology
China's tobacco planting area is large, and output is high but tobacco planting industry income is relatively low.Mainly utilized at present sound tobacco to be used for cigarette, the tobacco stem more than 10 times, cigarette muscle and offal and stacked or burning as discarded object, this has not only caused the wasting of resources, and has caused environmental pollution, becomes one of difficult problem that affects the tobacco business development.Utilize if tobacco waste is carried out " resource ", not only can turn waste into wealth, and can improve the national economy income, promote China's " two cigarettes " sound development of industry.
Contain abundant cellulose in tobacco.Cellulose can be widely used in the industries such as weaving, medicine, fermentation producing and ethanol, lactic acid, has very high social value.But due to its complicated space structure and fine and close degree of crystallinity, seriously hindered cellulosic industrial applications.
Summary of the invention
The object of the present invention is to provide a kind of cellulosic method of extracting from tobacco, the method operation energy consumption is low, pollutes littlely, and efficient is high, and cost is low.
For achieving the above object, technical scheme of the present invention is:
Extract cellulosic method from tobacco, specifically comprise the following steps:
The A solubilizing reaction
Add to be equivalent to doubly 1-butyl of tobacco quality 10-15-3-methylimidazole villaumite in tobacco, carry out sufficient solubilizing reaction under 80-100 ℃ of condition, get reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, get liquid, described liquid is cellulose solution;
The cellulosic acquisition of B
Adding volume in steps A gained cellulose solution is 3-5 aqueous medium doubly, filters after stirring is no less than 30 minutes, and the gained filter residue is cellulose.
Further, in steps A, described tobacco is tobacco.
Further, in steps A, the particle diameter of described tobacco is more than 20 orders.
Further, before solubilizing reaction, also comprise the pre-treatment step of tobacco, be specially: tobacco is soaked in aqueous medium be no less than 8 hours, carry out steam blasting and process, and carry out drying, get tobacco preliminary treatment material; The pressure that described steam blasting is processed is not less than 0.04Mpa, and the steam blasting time is no less than 60 seconds.
Further, in steps A, the mode of described Separation of Solid and Liquid is centrifugal, the centrifugal time to be no less than 5 minutes, and centrifugal speed is not less than 1500 rev/mins.
Further, in step B, described filter residue is washed with deionized water, and carry out vacuumize, get cellulose, described baking temperature is 50-80 ℃, and be 10-14 hour drying time.
Beneficial effect of the present invention is: the technique that the present invention adopts is simple, energy-conserving and environment-protective, process tobacco material by the steam blasting preconditioning technique and can reach the destruction cellulosic structure, can reach the purpose of activated cellulose again, can also effectively extract hemicellulose simultaneously, pollute little; Cellulose ion liquid dissolving after activation, not only solubility property is good, can also effectively reclaim ionic liquid, has saved production cost; Environmental pollution of the present invention is little, cost is lower, has enlarged greatly the scope of utilizing of crops tobacco wastes, has wide market prospects.Compare with traditional acid, alkali activation processing baccy fiber element, the steam blasting preliminary treatment has the effect that energy consumption is low, pollution is little, efficient is high, can reduce production costs significantly; First adopt steam blasting activation baccy fiber element, then use ion liquid dissolving, with the independent ion liquid dissolving cellulose of using, its dissolved efficiency has nearly improved 60%, has greatly improved dissolved efficiency.
Description of drawings
Fig. 1 is the SEM figure without the baccy fiber element of the tobacco of any processing, the tobacco material surface smoothing, and in order fine and close, the regular structure of this kind is unfavorable for the processing of 1-butyl-3-methylimidazole villaumite;
Fig. 2 is the large cellulosic SEM figure of the tobacco after the steam blasting pre-treatment and activation, make the separation of hemicellulose element due to the effect of steam blasting through material after the steam blasting activation processing, its surface texture becomes fluffy, this coarse surface texture makes ionic liquid process the contact area increase, and easily corrode the inside to the stalk material, destroy cellulosic crystalline texture;
Fig. 3 is that the SEM figure of tobacco is processed in the quick-fried activation of steam by ionic liquid, material mode of appearance after the quick-fried activation of steam is processed by ionic liquid, a large amount of holes appears in its surface, strip structure disappears, material has presented random structure fully, illustrates that its ionic liquid processing has destroyed its crystalline texture.After 1-butyl-3-methylimidazole villaumite is processed, the random structure of material increases its specific area greatly.
The specific embodiment
The tobacco of indication in the present invention also comprises offal, tobacco stem and tobacco leaf, discarded tobacco during especially tobacco produces, tobacco in following embodiment comes from Chongqing silver good fortune biological organic fertilizer Co., Ltd, for tobacco produces discarded object, its SEM schemes as shown in Figure 1, and its moisture is 7% of mass fraction.
Cellulose yield=(cellulose amount that obtains/cellulose total amount) * 100%.
Embodiment 1
Getting the 100g particle diameter is 20 purpose tobaccos, adds the 1-butyl of 10 times of quality that are equivalent to tobacco-3-methylimidazole villaumite, carries out the solubilizing reaction 4h time under 100 ℃ of conditions, get reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, get liquid, described liquid is cellulose solution; Adding volume in the gained cellulose solution is the deionized water of 3 times, stirs and filters after 30 minutes, and the gained filter residue is cellulose, and the cellulose quality is 9.6g, and the cellulose yield is 43.63%.
Embodiment 2
The NaOH that accurately takes 170g is dissolved in the distilled water of 510mL, is configured to mass concentration and is 25% NaOH solution.Taking the 120g particle diameter is that 20 purpose tobaccos are put into three-necked bottle, then to add the 500mL mass concentration be 25% NaOH solution, mechanical agitation reaction 1h, and reaction is washed suction filtration with distilled water after finishing, till being neutrality to suction filtration liquid.Filter residue is standby after 70 ℃ of vacuumize.Getting the 100g particle diameter is 20 purpose tobaccos, adds the 1-butyl of 10 times of quality that are equivalent to tobacco-3-methylimidazole villaumite, carries out the solubilizing reaction 4h time under 100 ℃ of conditions, get reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, get liquid, described liquid is cellulose solution; Adding volume in the gained cellulose solution is the deionized water of 5 times, stirs and filters after 30 minutes, and the gained filter residue is cellulose, and the cellulose quality is 19.2g, and the raw cellulose that is untreated has improved 43.64%, and the cellulose yield is 87.27%.
Embodiment 3
Taking the 120g particle diameter is that 20 purpose tobaccos are put into three-necked bottle, then to add the 500mL mass concentration be 10% hydrochloric acid solution, mechanical agitation reaction 1.5h, and reaction is washed suction filtration with distilled water after finishing, till being neutrality to suction filtration liquid.Filter residue is standby after 70 ℃ of vacuumize.Getting the 100g particle diameter is 20 purpose tobaccos, adds the 1-butyl of 10 times of quality that are equivalent to tobacco-3-methylimidazole villaumite, carries out the solubilizing reaction 4h time under 100 ℃ of conditions, get reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, get liquid, described liquid is cellulose solution; Adding volume in the gained cellulose solution is the deionized water of 3 times, stirs and filters after 30 minutes, and the gained filter residue is cellulose, and the cellulose quality is 19.5g, and the raw cellulose that is untreated has improved 45.01%, and the cellulose yield is 88.64%.
Embodiment 4
Taking the 100g particle diameter is that 20 purpose tobaccos are put into three-necked bottle, then to add the 500mL aqueous solution, ultrasonic power be 350w ultrasonic reaction 1.5h, and reaction is washed suction filtration with distilled water after finishing, till being neutrality to suction filtration liquid.Filter residue is standby after 70 ℃ of vacuumize.Getting the 100g particle diameter is 20 purpose tobaccos, adds the 1-butyl of 10 times of quality that are equivalent to tobacco-3-methylimidazole villaumite, carries out the solubilizing reaction 4h time under 100 ℃ of conditions, get reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, get liquid, described liquid is cellulose solution; Adding volume in the gained cellulose solution is the deionized water of 3 times, stirs and filters after 30 minutes, and the gained filter residue is cellulose, and the cellulose quality is 19.7g, and the raw cellulose that is untreated has improved 45.92%, and the cellulose yield is 89.55%
Embodiment 5
Getting the 100g particle diameter is 30 purpose tobaccos, add the 1-butyl of 10 times of quality that are equivalent to tobacco-3-methylimidazole villaumite, carry out solubilizing reaction under 80 ℃ of conditions, get reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, the mode of described Separation of Solid and Liquid is centrifugal, the centrifugal time is 5 minutes, 1500 rev/mins of centrifugal speed are got liquid, and described liquid is cellulose solution; Adding volume in the gained cellulose solution is the deionized water of 3 times, stirs and filters after 30 minutes, and the gained filter residue is cellulose; Described filter residue washs with deionized water, and carries out vacuumize, gets cellulose, and described baking temperature is 50 ℃, and be 10 hours drying time, and the cellulose quality is 9.8g, and the cellulose yield is 44.54%.
Embodiment 6
Getting the 100g particle diameter is 60 purpose tobaccos, add the 1-butyl of 15 times of quality that are equivalent to tobacco-3-methylimidazole villaumite, carry out the solubilizing reaction 4h time under 100 ℃ of conditions, get reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, the mode of described Separation of Solid and Liquid is centrifugal, the centrifugal time is 8 minutes, 4000 rev/mins of centrifugal speed are got liquid, and described liquid is cellulose solution; Adding volume in the gained cellulose solution is the deionized water of 3 times, stirs and filters after 240 minutes, and the gained filter residue is cellulose; Described filter residue is washed with deionized water, and carry out vacuumize, get cellulose, described baking temperature is 80 ℃, and be 14 hours drying time.After dry, the cellulose quality is 9.3g, and the cellulose yield is 42.27%
Embodiment 7
Embodiment 7 compares with embodiment 6, and before solubilizing reaction, many step tobacco pre-treatment step are specially: tobacco was soaked in aqueous medium 8 hours, carried out steam blasting and process, and carry out drying, get tobacco preliminary treatment material, its SEM figure sees Fig. 2 for details; The pressure that described steam blasting is processed is 0.04Mpa, 60 seconds steam blasting time, get cellulose after drying, and see Fig. 3 for details, cellulosic quality is 21.3g, and the raw cellulose that is untreated has improved 54.55%, and the cellulose yield is 96.82%.
Embodiment 8
Embodiment 8 compares with embodiment 6, and before solubilizing reaction, many step tobacco pre-treatment step are specially: tobacco was soaked in aqueous medium 12 hours, carried out steam blasting and process, and carry out drying, get tobacco preliminary treatment material; The pressure that described steam blasting is processed is 0.26Mpa, and 180 seconds steam blasting time, dry rear cellulose quality is 21.5g, and the raw cellulose that is untreated has improved 55.46%, and the cellulose yield is 97.73%.
Utilize traditional acid, alkali activating technology also to need the waste liquid after processing is processed, increased production cost, and be unfavorable for that environment and ecology develops in a healthy way.The ultrasonic activation technology is because ultrasonic technique easily produces cavity effect, and the easy dead angle that produces that produces, and is unfavorable for the production of large industrialized.The steam blasting activating technology utilizes steam to reach the purpose of activated cellulose, has not only saved production cost, has reached the purpose of efficient activation, also helps environment and ecological protection.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although by invention has been described with reference to the preferred embodiments of the present invention, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (2)
1. extract cellulosic method from tobacco, it is characterized in that, getting particle diameter is 60 purpose tobaccos, soaked 12 hours in aqueous medium, carry out steam blasting and process, and carry out drying, get tobacco preliminary treatment material, the pressure that described steam blasting is processed is 0.26MPa, 180 seconds steam blasting time; Add the 1-butyl that is equivalent to 15 times of tobacco qualities-3-methylimidazole villaumite in tobacco preliminary treatment material, carry out solubilizing reaction 4h under 100 ℃ of conditions, get reactant liquor, described reactant liquor is carried out Separation of Solid and Liquid, the mode of described Separation of Solid and Liquid is that centrifugal, the centrifugal time is 8 minutes, 4000 rev/mins of centrifugal speed, get liquid, described liquid is cellulose solution; Adding volume in the gained cellulose solution is the deionized water of 3 times, stirs and filters after 240 minutes, and the gained filter residue is cellulose; Described filter residue is washed with deionized water, and carry out vacuumize, get cellulose, described baking temperature is 80 ℃, and be 14 hours drying time.
2. according to claim 1ly extract cellulosic method from tobacco, it is characterized in that, described tobacco is that tobacco produces discarded object.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110248519 CN102304865B (en) | 2011-08-26 | 2011-08-26 | Method for extracting cellulose from tobacco |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110248519 CN102304865B (en) | 2011-08-26 | 2011-08-26 | Method for extracting cellulose from tobacco |
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| CN102304865A CN102304865A (en) | 2012-01-04 |
| CN102304865B true CN102304865B (en) | 2013-06-12 |
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| CN 201110248519 Expired - Fee Related CN102304865B (en) | 2011-08-26 | 2011-08-26 | Method for extracting cellulose from tobacco |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102733221B (en) * | 2012-02-23 | 2015-06-24 | 重庆恒远晋通科技有限公司 | Method for recycling lignin and cellulose in tobacco waste |
| CN102733222A (en) * | 2012-02-23 | 2012-10-17 | 重庆恒远晋通科技有限公司 | Method for extracting cellulose from tobacco waste by zinc chloride process |
| UA115782C2 (en) | 2012-03-28 | 2017-12-26 | Філіп Морріс Продактс С.А. | Liquid tobacco compositions |
| GB201221209D0 (en) * | 2012-11-26 | 2013-01-09 | British American Tobacco Co | Treatment of tobacco material |
| CN104087621A (en) * | 2014-07-25 | 2014-10-08 | 重庆恒远晋通科技有限公司 | Fermentation production method for liquor by utilizing tobacco waste |
| CN106368034A (en) * | 2016-11-14 | 2017-02-01 | 哈尔滨工业大学 | Method for extracting cellulose from traditional Chinese medicine dregs and application of cellulose |
| CN115487778B (en) * | 2022-10-13 | 2024-07-12 | 湖南口味王集团有限责任公司 | Biochar and preparation method thereof |
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| US8182557B2 (en) * | 2007-02-06 | 2012-05-22 | North Carolina State University | Use of lignocellulosics solvated in ionic liquids for production of biofuels |
| CN101649571B (en) * | 2009-08-31 | 2011-06-08 | 中国科学院广州化学研究所 | Method for dissolving and extracting cellulose in bagasse |
| CN101880411B (en) * | 2010-02-23 | 2012-04-18 | 广西壮族自治区化工研究院 | Method for preparing functional regenerated cellulose membrane from bagasse cellulose |
| CN101871020B (en) * | 2010-07-14 | 2012-05-30 | 河南科技大学 | Method for preparing wood sugar, glucose and lignin with ionic liquid controllable hydrolytic wood fiber raw material |
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