CN102268827A - Method for extracting celluloses from tobaccos based on ferric chloride pretreatment - Google Patents
Method for extracting celluloses from tobaccos based on ferric chloride pretreatment Download PDFInfo
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Abstract
The invention relates to a process for extracting celluloses from tobaccos. A pretreatment method of the tobaccos is characterized by subjecting the tobacco materials to react with a ferric chloride solution at a concentration of 0.2-0.6mol/L at 120-140 DEG C for at least 20 minutes to obtain a tobacco pretreatment liquid. The process comprises the following steps: washing the tobacco pretreatment liquid until the tobacco pretreatment liquid is neutral and filtering and drying the neutral tobacco pretreatment liquid to obtain neutral tobacco pretreatment materials; adding 1-butyl-3-methyl-imidazolium chloride with mass being equal to 10-15 times the mass of the tobaccos to the neutral tobacco pretreatment materials to undergo a full dissolution reaction at 80-100 DEG C to obtain a reaction liquid, carrying out solid-liquid separation on the reaction liquid and obtaining the liquid, namely the cellulose solution; and adding an aqueous medium to the cellulose solution and carrying out filtration after stirring for at least 30 minutes, thus obtaining the filter residues, namely the cellulose. Or the process is characterized by filtering the tobacco pretreatment liquid to obtain a filtrate, adjusting the pH value of the filtrate to 3.0-5.0, generating solid precipitates and carry out liquid-solid separation on the solid precipitates to obtain the solid precipitates, namely hemicelluloses. The process has the advantages of low cost, high yield and environment friendliness.
Description
Technical field
The present invention relates to chemical field, particularly from plant, extract the technology of cellulose and hemicellulose.
Background technology
China's tobacco planting area is big, output height but tobacco planting industry has mainly been utilized sound tobacco to be used for cigarette, the tobacco stem more than 10 times, cigarette muscle and offal at present to stack or burning as discarded object, this has not only caused the wasting of resources, and caused environmental pollution, become one of difficult problem that influences 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 the tobacco.Cellulose can be widely used in industries such as weaving, medicine, fermentation producing and ethanol, lactic acid, has very high social value.But because its complicated spatial structure and fine and close degree of crystallinity have seriously hindered cellulosic industrial applications.
Hemicellulose in the tobacco is meant the polysaccharide mixture of combining closely with cellulose in the tobacco cell wall, can be used for preparing yeast or ribonucleic acid, is derivatized to inosine list phosphoric acid system and the acid of guanosine egg phosphatide again, can be used as flavor enhancement, anticancer or antiviral reaching.
Summary of the invention
One of purpose of the present invention is to provide a preprocess method that grows tobacco, and this method can realize realizing simultaneously the purpose of degradation of hemicellulose and activated cellulose.
For achieving the above object, technical scheme of the present invention is:
The preprocess method of tobacco is that the ferric chloride solution of 0.2-0.6mol/L is that reaction was not less than 20-40 minute under the 120-140 ℃ of condition in temperature with concentration with tobacco, the tobacco pretreatment fluid.
Further, be that the ferric chloride solution of 0.4mol/L is that reaction was not less than 30 minutes under the 120-140 ℃ of condition in temperature with tobacco with concentration, the tobacco pretreatment fluid.
Further, described tobacco particle diameter is more than 20 orders.
Two of purpose of the present invention is to provide the material that grows tobacco, and this tobacco material can be used for extracting cellulose or hemicellulose.
For achieving the above object, technical scheme of the present invention is:
The tobacco pretreatment fluid of the preprocess method gained of described tobacco.
Three of purpose of the present invention is to provide a kind of cellulosic extracting method, and this method energy consumption is little, and cost is low.
For achieving the above object, technical scheme of the present invention is:
Extract cellulosic method based on described tobacco, specifically may further comprise the steps:
The A washing
Described tobacco pretreatment fluid washing to neutral, is filtered, and drying gets neutral tobacco preliminary treatment material;
The B solubilizing reaction
Be equivalent to tobacco quality 10-15 1-butyl-3-methylimidazole villaumite doubly in the adding of the neutral tobacco preliminary treatment of steps A gained material, under 80-100 ℃ of condition, carry out sufficient solubilizing reaction, 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 C
Add aqueous medium in step B gained cellulose solution, the volume ratio of described cellulose solution and aqueous medium is 1:3-5, filters after stirring is no less than 30 minutes, and the gained filter residue is a cellulose.
Further, in step B, 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 C, described filter residue is washed with deionized water, and carry out vacuumize, get cellulose, described baking temperature is 50-80 ℃.
Further, in step C, add in step B gained cellulose solution and be equivalent to cellulose solution volume 3-5 deionized water doubly, filter after stirring is no less than 240 minutes, the gained filter residue is a cellulose.
Four of purpose of the present invention is to provide a kind of method of extracting hemicellulose, and the waste liquid that this method is extracted behind the cellulose with tobacco is a raw material, environmental protection.
For achieving the above object, technical scheme of the present invention is:
Based on the method for described tobacco pretreatment fluid extraction hemicellulose, described tobacco pretreatment fluid is filtered, get filtrate, described filtrate is regulated pH value 3.0-5.0, treat fully to produce solid precipitation, carry out liquid-solid separation, described solid precipitation is a hemicellulose.
Further, described tobacco pretreatment fluid is filtered, get filtrate, described filtrate is regulated pH value 3.0-5.0, produce solid precipitation, carry out liquid-solid separation, collect solid, the liquid after the liquid-solid separation precipitates with ethanol precipitation, collecting precipitation, described solid precipitation and described precipitation are merged, must merge thing, described merging thing is a hemicellulose.
Beneficial effect of the present invention is: the iron chloride preliminary treatment is a kind of effective preprocess method, and its energy consumption is low, and is little to ambient influnence.After the preliminary treatment of the plain raw material process of baccy fiber iron chloride, the hemicellulose degraded, structure is destroyed, and can reach the purpose of effective activated cellulose simultaneously.The advantage of selective chlorination iron pre-treatment and activation baccy fiber element of the present invention mainly contains: 1 adopts the ion liquid dissolving cellulose separately, dissolution rate is low, but after the activation of iron chloride technology, baccy fiber element destructurized, more help ion liquid infiltration, improved cellulosic dissolution rate, the cellulose dissolution rate has on average improved 50%; 2 compare with traditional handicraft, and iron chloride and treatment technology have less energy consumption, low cost and other advantages; 3 metal ions can excite the generation free radical, can effectively destroy the link between hemicellulose, cellulose and the lignin, destroy in its molecule and intermolecular structure; 4 chlorions also have the ability that promotes ion liquid dissolving baccy fiber element.
Iron chloride can be got rid of the hemicellulose more than 90% after handling tobacco waste, and required mild condition, and ferric chloride solution can be reused after reclaiming.
Description of drawings
The infrared spectrogram figure of Fig. 1 baccy fiber element, wherein a representative is without the tobacco of any processing; B represent after the ferric chloride solution pre-treatment and activation tobacco; C is represented as the ferric chloride solution activation after the regenerated cellulose behind the ion liquid dissolving.
The specific embodiment
The tobacco of indication among the present invention, also comprise offal, tobacco stem and tobacco leaf, discarded tobacco during especially tobacco produces, the tobacco among the following embodiment come from Chongqing silver good fortune biological organic fertilizer Co., Ltd, for tobacco produces discarded object, its moisture is 7% of a mass fraction.
Cellulose amount/cellulose the total amount of cellulose yield=obtain) * 100%; Hemicellulose amount/hemicellulose the total amount of hemicellulose yield=obtain) * 100%.
Precipitation with alcohol hemicellulose principle: hemicellulose is the most complicated component in the cell membrane of timber and non-wood plant.They connect with hemicellulose by hydrogen bond, connect with covalent bond (mainly being the benzyl ehter bond) with lignin, connect with ester bond with acetyl group unit and hydroxycinnamic acid.Hemicellulose is under sour environment, and hydrogen bond ruptures, and hemicellulose is similar to the low mass molecule alcohol class, and according to the similar compatibility principle, hemicellulose is dissolved in the ethanol, reclaims ethanol by rotary evaporation again, obtains the hemicellulose solid.
The preparation of embodiment 1 tobacco pretreatment fluid
The ferric chloride solution that with tobacco with concentration is 0.2mol/L is that reaction is 40 minutes under 120 ℃ of conditions in temperature, the tobacco pretreatment fluid.
The preparation of embodiment 2 tobacco pretreatment fluids
The ferric chloride solution that with tobacco material with concentration is 0.6mol/L is that reaction is 20 minutes under 140 ℃ of conditions in temperature, must the tobacco pretreatment fluid.
The preparation of embodiment 3 tobacco pretreatment fluids
The tobacco material is that the ferric chloride solution of 0.4mol/L is that reaction is 30 minutes under 130 ℃ of conditions in temperature with concentration, gets the tobacco pretreatment fluid.
Embodiment 4 cellulosic extractions
Be divided into is 4 groups, the 1st group is the tobacco pretreatment fluid of embodiment 1 preparation, the 2nd group is the tobacco pretreatment fluid of embodiment 2 preparations, the 3rd group is the tobacco pretreatment fluid of embodiment 3 preparations, the 4th group for being that 100 ℃ conditions under reaction be 60 minute with deionized water in temperature with tobacco, must the tobacco pretreatment fluid.It is raw material that above-mentioned tobacco pretreatment fluid all is ground into after 20 orders sieve with the tobacco waste residue.
Cellulosic extracting method: granular size tobacco between the 40-60 order is added distilled water according to liquid-solid mass ratio 1:1 spend the night.Be 2.2Mpa at steam blasting pressure next day, and dimension is to carry out the steam blasting preliminary treatment under 9 minutes the condition pressure time, collects the material after steam blasting is handled, 105 ℃ of dry for standby.Material after will drying then adopts the method for water/pure extracting to handle, with realize hemicellulose, lignin with component separate.
Concrete water/pure processing method is: with the oven dry tobacco through 75 ℃ of distilled water according to liquid-solid mass ratio 30:100, adverse current extracting 6 times, filter rear filtrate and be used to extract hemicellulose, filter residue is that 70% alcohol is according to solid-to-liquid ratio 1:50 suction filtration behind 160 ℃ of following oil bath 1h through volume fraction, filter residue is a cellulose, and filtrate being used to extracted lignin.Gained cellulose quality first group is for 18.3g, and second group is 19.2g, and the 3rd group is 18.5g, and the 4th group is 12.4g.
Above-mentioned cellulose detects cellulose through infrared spectrum.By shown in Figure 1, contain more polydextrose and xylan-arabinose-glucuronic acid in the tobacco, the deformation vibration of-CH2-and stretching vibration cause at 1 400 cm
-1, 2 900 cm
-1Near tangible absworption peak is arranged; The stretching vibration of C=O causes at 1 600 cm
-1Near absworption peak; The stretching vibration of C-O-C key influences 1 100 cm
-1Near bands of a spectrum.By infrared spectrogram as can be known, tobacco material is at 1100cm
-1, 1 400 cm
-1, 3100cm
-1Near tangible absworption peak is arranged, and sample after ferric chloride solution is handled at 1 400 cm
-1, 1 600 cm
-1, 3 400 cm
-1Near absworption peak weaken, promptly-absworption peak of CH2-, C=O, O-H weakens, illustrate with xylan-arabinose-glucuronic acid to be that the hemicellulose of representative decomposes in the ferric chloride solution processing procedure; Through after the ferric chloride solution activation again the sample after ionic liquid is handled at 1100cm
-1Near peak intensity reduces, and shows that the C-O-C key has fracture in various degree, and the C-O-C key is the main associative key on the cellulose chain, and its fracture will make cellulosic degree of polymerization decrease to some degree.Simultaneously at 1000 cm
-1The bands of a spectrum at place obviously strengthen.
Embodiment 5 cellulosic extractions
Be divided into is 4 groups, the 1st group is the tobacco pretreatment fluid of embodiment 1 preparation, the 2nd group is the tobacco pretreatment fluid of embodiment 2 preparations, the 3rd group is the tobacco pretreatment fluid of embodiment 3 preparations, the 4th group for being that 100 ℃ conditions under reaction be 60 minute with deionized water in temperature with tobacco, must the tobacco pretreatment fluid.It is raw material that above-mentioned tobacco pretreatment fluid all is ground into after 20 orders sieve with the tobacco waste residue.
Cellulosic extracting method: 4 groups of tobacco pretreatment fluids are spent deionised water to neutral, filter, reclaim ferric chloride solution, 80 ℃ of vacuumizes of filter residue 12 hours, get neutral tobacco preliminary treatment material, 1-butyl-3-methylimidazole the villaumite that in neutral tobacco preliminary treatment material, adds 10 times of quality being equivalent to neutral tobacco preliminary treatment material, under 80 ℃ of conditions, carry out solubilizing reaction, 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; The adding volume is 3 times a deionized water in the gained cellulose solution, stirs and filters after 30 minutes, and the gained filter residue is a 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.Gained cellulose quality first group is for 18.5g, and second group is 19.6g, and the 3rd group is 18.3g, and the 4th group is 12.7g.
Embodiment 6 cellulosic extractions
Be divided into is 4 groups, the 1st group is the tobacco pretreatment fluid of embodiment 1 preparation, the 2nd group is the tobacco pretreatment fluid of embodiment 2 preparations, the 3rd group is the tobacco pretreatment fluid of embodiment 3 preparations, the 4th group is that tobacco is expected that be that reaction is 60 minutes under 100 ℃ of conditions with deionized water in temperature, gets the tobacco pretreatment fluid.It is raw material that above-mentioned tobacco pretreatment fluid all is ground into after 40 orders sieve with the tobacco waste residue.
Cellulosic extracting method: 4 groups of tobacco pretreatment fluids are spent deionised water to neutral, filter, reclaim ferric chloride solution, 80 ℃ of vacuumizes of filter residue 12 hours, get neutral tobacco pretreatment fluid preliminary treatment material, 1-butyl-3-methylimidazole the villaumite that in neutral tobacco pretreatment fluid preliminary treatment material, adds 15 times of quality being equivalent to neutral tobacco pretreatment fluid preliminary treatment material, under 100 ℃ of conditions, carry out the solubilizing reaction 4h time, 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; The adding volume is 5 times a deionized water in the gained cellulose solution, stirs and filters after 240 minutes, and the gained filter residue is a 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.Gained cellulose quality first group is for 18.7g, and second group is 20.6g, and the 3rd group is 19.3g, and the 4th group is 12.5g.
The extracting method of embodiment 7 hemicelluloses
Be divided into is 4 groups, the 1st group is the tobacco pretreatment fluid of embodiment 1 preparation, the 2nd group is the tobacco pretreatment fluid of embodiment 2 preparations, the 3rd group is the tobacco pretreatment fluid of embodiment 3 preparations, the 4th group is that tobacco is expected that be that reaction is 60 minutes under 100 ℃ of conditions with deionized water in temperature, gets the tobacco pretreatment fluid.It is raw material that above-mentioned tobacco pretreatment fluid all is ground into after 60 orders sieve with the tobacco waste residue.
The extracting method of hemicellulose: described tobacco pretreatment fluid is regulated pH value 3.0, and centrifugation liquid and solid are collected solid, described liquid precipitates with ethanol precipitation, and collecting precipitation merges described solid and described precipitation, must merge thing, described merging thing is a hemicellulose.Gained hemicellulose quality first group is for 12.7g, and second group is 13.6g, and the 3rd group is 12.3g, and the 4th group is 10.5g
The extracting method of embodiment 8 hemicelluloses
Be divided into is 4 groups, the 1st group is the tobacco pretreatment fluid of embodiment 1 preparation, the 2nd group is the tobacco pretreatment fluid of embodiment 2 preparations, the 3rd group is the tobacco pretreatment fluid of embodiment 3 preparations, the 4th group is that tobacco is expected that be that reaction is 40 minutes under 100 ℃ of conditions with deionized water in temperature, gets the tobacco pretreatment fluid.It is raw material that above-mentioned tobacco pretreatment fluid all is ground into after 60 orders sieve with the tobacco waste residue.
The extracting method of hemicellulose: described tobacco pretreatment fluid is regulated pH value 5.0, and centrifugation liquid and solid are collected solid, described liquid precipitates with ethanol precipitation, and collecting precipitation merges described solid and described precipitation, must merge thing, described merging thing is a hemicellulose.Gained hemicellulose quality first group is for 12.9g, and second group is 13.5g, and the 3rd group is 12.7g, and the 4th group is 11.5g.
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 the spirit and scope of the present invention that do not depart from appended claims and limited.
Claims (10)
1. the preprocess method of tobacco is characterized in that, is that the ferric chloride solution of 0.2-0.6mol/L is that reaction was not less than 20 minutes under the 120-140 ℃ of condition in temperature with concentration with tobacco, gets the tobacco pretreatment fluid.
2. the preprocess method of tobacco according to claim 1 is characterized in that, is that the ferric chloride solution of 0.4mol/L is that reaction was not less than 30 minutes under the 120-140 ℃ of condition in temperature with concentration with tobacco, gets the tobacco pretreatment fluid.
3. the preprocess method of tobacco according to claim 1 is characterized in that, described tobacco particle diameter is more than 20 orders.
4. the tobacco pretreatment fluid of the preprocess method gained of each described tobacco among the claim 1-3.
5. extract cellulosic method based on the described tobacco of claim 4, it is characterized in that, specifically may further comprise the steps:
The A washing
Described tobacco pretreatment fluid washing to neutral, is filtered, and drying gets neutral tobacco preliminary treatment material;
The B solubilizing reaction
Be equivalent to tobacco quality 10-15 1-butyl-3-methylimidazole villaumite doubly in the adding of the neutral tobacco preliminary treatment of steps A gained material, under 80-100 ℃ of condition, carry out sufficient solubilizing reaction, 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 C
Add aqueous medium in step B gained cellulose solution, the volume ratio of described cellulose solution and aqueous medium is 1:3-5, filters after stirring is no less than 30 minutes, and the gained filter residue is a cellulose.
6. tobacco pretreatment fluid according to claim 5 extracts cellulosic method, it is characterized in that, in step B, 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.
7. tobacco pretreatment fluid according to claim 5 extracts cellulosic method, it is characterized in that, in step C, described filter residue is washed with deionized water, and carries out vacuumize, gets cellulose, and described baking temperature is 50-80 ℃.
8. tobacco pretreatment fluid according to claim 5 extracts cellulosic method, it is characterized in that, in step C, in step B gained cellulose solution, add and be equivalent to cellulose solution volume 3-5 deionized water doubly, stirring is filtered after being no less than 240 minutes, and the gained filter residue is a cellulose.
9. extract the method for hemicellulose based on the described tobacco pretreatment fluid of claim 4, it is characterized in that, described tobacco pretreatment fluid is filtered, get filtrate, described filtrate is regulated pH value 3.0-5.0, treat fully to produce solid precipitation, carry out liquid-solid separation, described solid precipitation is a hemicellulose.
10. tobacco pretreatment fluid according to claim 9 extracts the method for hemicellulose, it is characterized in that, described tobacco pretreatment fluid is filtered, get filtrate, described filtrate is regulated pH value 3.0-5.0, produce solid precipitation, carry out liquid-solid separation, collect solid, liquid after the liquid-solid separation precipitates with ethanol precipitation, and collecting precipitation merges described solid precipitation and described precipitation, must merge thing, described merging thing is a hemicellulose.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102733221A (en) * | 2012-02-23 | 2012-10-17 | 重庆恒远晋通科技有限公司 | Method for recycling lignin and cellulose in tobacco waste |
| CN102733218A (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 based on aluminium chloride process |
| 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 |
| CN102731475A (en) * | 2012-02-23 | 2012-10-17 | 重庆恒远晋通科技有限公司 | Method for recycling nicotine and hemicellulose in tobacco waste |
| CN109627347A (en) * | 2018-12-12 | 2019-04-16 | 怀化学院 | The preprocess method of cellulose |
| CN109722932A (en) * | 2019-02-21 | 2019-05-07 | 南京农业大学 | A method of extracting agricultural stalk class waste cellulose |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102733221A (en) * | 2012-02-23 | 2012-10-17 | 重庆恒远晋通科技有限公司 | Method for recycling lignin and cellulose in tobacco waste |
| CN102733218A (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 based on aluminium chloride process |
| 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 |
| CN102731475A (en) * | 2012-02-23 | 2012-10-17 | 重庆恒远晋通科技有限公司 | Method for recycling nicotine and hemicellulose in tobacco waste |
| 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 |
| CN109627347A (en) * | 2018-12-12 | 2019-04-16 | 怀化学院 | The preprocess method of cellulose |
| CN109722932A (en) * | 2019-02-21 | 2019-05-07 | 南京农业大学 | A method of extracting agricultural stalk class waste cellulose |
| CN109722932B (en) * | 2019-02-21 | 2021-08-03 | 南京农业大学 | Method for extracting cellulose from agricultural straw waste |
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Application publication date: 20111207 |