CN108330723A - A method of extracting cellulose using the false indigo of salt-soda soil plantation - Google Patents
A method of extracting cellulose using the false indigo of salt-soda soil plantation Download PDFInfo
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- CN108330723A CN108330723A CN201711455090.3A CN201711455090A CN108330723A CN 108330723 A CN108330723 A CN 108330723A CN 201711455090 A CN201711455090 A CN 201711455090A CN 108330723 A CN108330723 A CN 108330723A
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- false indigo
- salt
- mixed liquor
- cellulose
- soda soil
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/001—Modification of pulp properties
- D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
- D21C9/004—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives inorganic compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/001—Modification of pulp properties
- D21C9/007—Modification of pulp properties by mechanical or physical means
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/1084—Bleaching ; Apparatus therefor with reducing compounds
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- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The present invention relates to a kind of methods that cellulose is extracted in cellulose extractive technique field more particularly to false indigo using salt-soda soil plantation, including pretreatment, Acid treatment, soda boiling processing, bleaching, microwave treatment.The yield and purity of cellulose are improved using the extracting method of the present invention.
Description
Technical field
The present invention relates to chemical fiber fields more particularly to a kind of false indigo using salt-soda soil plantation to extract fiber
The method of element.
Background technology
False indigo is a kind of perennial pulse family machaka, and since it has growth fast, reproductive capacity is strong, wide adaptability, resistance to
The characteristics such as saline-alkali water is wet improve seeds with green manure and alkaline land soil extensively in strand and saline-alkali wetland area.
The main chemical compositions of false indigo are cellulose, hemicellulose, lignin ash content, therefore can be used to make by false indigo
Starch papermaking, fiberboard and composite plate.There is the process of a large amount of extraction celluloses in the prior art, but is extracted from false indigo
The technique of cellulose has not been reported.
Invention content
The technical problem to be solved by the present invention is to：In view of the deficienciess of the prior art, offer is a kind of to utilize salt-soda soil
The method of the false indigo extraction cellulose of plantation, the yield of cellulose can be improved using this method.
In order to solve the above technical problems, the technical scheme is that：
A method of cellulose being extracted using the false indigo of salt-soda soil plantation, the described method comprises the following steps：
(1) it pre-processes：By false indigo peeling, crushing, sieving, drying, cooling, false indigo wood powder is obtained；
(2) Acid treatment：False indigo wood powder in step (1) is taken, the mixed of organic solvent-organic acid-surfactant is added
Close liquid, stirring, heating boiling, cooling, filtering after the filter residue of collection is rinsed repeatedly with organic solvent, then are rinsed with deionized water；
(3) soda boiling is handled：Lye-is added into the filter residue rinsed by organic solvent flushing, deionized water in step (2)
The mixed liquor of organic solvent heats boiling, solid-state filtrate is collected in filtering by being ultrasonically treated；
(4) bleaching：Solid-state filtrate in step (3) is taken, organic acid-bleaching agent mixed liquor is added and is bleached, obtains
It is starched in vain to false indigo；
(5) microwave treatment：It takes false indigo in step (4) to starch addition calcium hydroxide solution in vain, filters, dry after microwave treatment
Obtain false indigo cellulose.
As an improvement technical solution, in step (2) in the mixed liquor of organic solvent-organic acid-surfactant
Organic solvent is ethyl alcohol, n-butanol or isopropanol；Organic acid is citric acid, tartaric acid or oxalic acid；Surfactant is dodecane
Base benzene sulfonic acid sodium salt or Tween-60.
As a kind of perferred technical scheme, the mixed liquor of the organic solvent-organic acid-surfactant is second
The mixed liquor of alcohol/isopropanol-tartaric acid-Tween-60.
As a kind of further preferred technical solution, the volumetric concentration of the ethyl alcohol is 65%-80%.
As an improvement technical solution, the temperature of boiling is 120-180 DEG C in step (2), and the time of boiling is 1-
3h。
As a kind of perferred technical scheme, temperature when step (3) is ultrasonically treated is 80-120 DEG C, time 1-4h,
The power of ultrasonic wave is 200-400w.
As an improvement technical solution, the mixed liquor of lye-organic solvent in step (3) is 0.5-1mol hydrogen-oxygens
Change the mixed liquor of sodium solution/potassium hydroxide solution-isopropanol.
As an improvement technical solution, the mixed liquor of organic acid-bleaching agent is-four acetyl second of acetic acid in step (4)
The mixed liquor of diamines/sodium hypochlorite/sodium sulfite.
As a kind of perferred technical scheme, bleaching temperature is 60-100 DEG C in step (4), bleaching time 1-2h.
As an improvement technical solution, the power of microwave treatment is 200-300w, temperature 80-120 in step (5)
℃。
After using above-mentioned technical proposal, the beneficial effects of the invention are as follows：
Compared with prior art, the present invention mainly has the following advantages：
(1) using the false indigo of salt-soda soil plantation as raw material, by Acid treatment after crushing false indigo, second is added in the present invention
Alcohol-tartaric acid-Tween-60 mixed liquor, by thermophilic digestion, ethyl alcohol-tartaric acid-Tween-60 enters cell interior, and and cell
Tissue comes into full contact with, and increases the contact area of lignin and mixed liquor so that a large amount of lignin are degraded and are dissolved in ethyl alcohol, together
When also degrade part hemicellulose；The mixed liquor for adding sodium hydroxide solution/potassium hydroxide solution-isopropanol, by super
Sonication and boiling processing, can destroy the cross-linked structure between cellulose and hemicellulose, make a large amount of hemicellulose degradations and molten
In isopropanol；By bleaching, microwave treatment, delignification and hemicellulose are further removed, fiber is substantially increased
The yield of plain product.
(2) present invention can effectively be removed delignification and hemicellulose, be reduced molten using microwave, ultrasonic-assistant solvent method
The usage amount of agent alleviates the pollution to environment.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Example 1
A method of cellulose being extracted using the false indigo of salt-soda soil plantation, is included the following steps：
(1) it pre-processes：By false indigo peeling, crushing, sieving, drying, cooling, false indigo wood powder is obtained；
(2) Acid treatment：False indigo wood powder in step (1) is taken, the organic molten of false indigo wood powder 8 times of volumes of weight is added
(volumetric concentration is the mixed liquor of 65% ethyl alcohol-tartaric acid-Tween-60, and second to the mixed liquor of agent-organic acid-surfactant
The volume ratio of alcohol, tartaric acid and Tween-60 is 1:1:0.5) it, stirs, heat temperature to 120 DEG C, boiling 1h, cooling, filtering is collected
Filter residue rinsed repeatedly with organic solvent after, then rinsed with deionized water；
(3) soda boiling is handled：Filter residue is added into the filter residue rinsed by organic solvent flushing, deionized water in step (2)
Lye-the organic solvent of 5 times of volumes of weight mixed liquor (0.5mol sodium hydroxide solutions/potassium hydroxide solution-isopropanol it is mixed
Close liquid, and the volume ratio 1 of lye and isopropanol:1), heating temperature is to 80 DEG C, under conditions of the power of ultrasonic wave is 200w, surpasses
Sonication 1h is again heated to 130 DEG C of boiling 1h, and solid-state filtrate is collected in filtering；
(4) bleaching：Solid-state filtrate in step (3) is taken, the organic acid-of solid-state filtrate 5 times of volumes of weight is added
Bleaching agent (acetic acid-tetraacetyl ethylene diamine mixed liquor) mixed liquor, most 60 DEG C of heating temperature bleach 1h, obtain false indigo and starch in vain；
(5) microwave treatment：False indigo in step (4) is taken to starch in vain, according to volume ratio 1:It is molten that calcium hydroxide is added in 2 ratio
Liquid is 200w in power, and temperature is handled under conditions of being 80 DEG C, filtered, and drying obtains false indigo cellulose.
The yield of false indigo cellulose is 78.56% under this process conditions.
Example 2
A method of cellulose being extracted using the false indigo of salt-soda soil plantation, is included the following steps：
(1) it pre-processes：By false indigo peeling, crushing, sieving, drying, cooling, false indigo wood powder is obtained；
(2) Acid treatment：False indigo wood powder in step (1) is taken, the organic molten of false indigo wood powder 10 times of volumes of weight is added
(volumetric concentration is the mixed liquor of 70% ethyl alcohol-tartaric acid-Tween-60, and second to the mixed liquor of agent-organic acid-surfactant
The volume ratio of alcohol, tartaric acid and Tween-60 is 2:1:1) it, stirs, heat temperature to 135 DEG C, boiling 1.8h, cooling, filtering is collected
Filter residue rinsed repeatedly with organic solvent after, then rinsed with deionized water；
(3) soda boiling is handled：Filter residue is added into the filter residue rinsed by organic solvent flushing, deionized water in step (2)
Lye-the organic solvent of 8 times of volumes of weight mixed liquor (mixed liquor of 0.6mol sodium hydroxide solutions-isopropanol, and lye with
The volume ratio 2 of isopropanol:1), heating temperature is to 90 DEG C, under conditions of the power of ultrasonic wave is 280w, is ultrasonically treated 2h, then add
Solid-state filtrate is collected in heat to 138 DEG C of boiling 1.5h, filtering；
(4) bleaching：Solid-state filtrate in step (3) is taken, the organic acid-of solid-state filtrate 8 times of volumes of weight is added
Bleaching agent (mixed liquor of acetic acid-sodium hypochlorite) mixed liquor, most 80 DEG C of heating temperature bleach 1.5h, obtain false indigo and starch in vain；
(5) microwave treatment：False indigo in step (4) is taken to starch in vain, according to volume ratio 1:It is molten that calcium hydroxide is added in 5 ratio
Liquid is 260w in power, is handled under the conditions of at a temperature of 90 °C, filter, drying obtains false indigo cellulose.
The yield of false indigo cellulose is 79.25% under the process conditions
Example 3
A method of cellulose being extracted using the false indigo of salt-soda soil plantation, is included the following steps：
(1) it pre-processes：By false indigo peeling, crushing, sieving, drying, cooling, false indigo wood powder is obtained；
(2) Acid treatment：False indigo wood powder in step (1) is taken, the organic molten of false indigo wood powder 12 times of volumes of weight is added
Mixed liquor (the mixed liquor of isopropanol-tartaric acid-Tween-60, and ethyl alcohol, tartaric acid and spit of agent-organic acid-surfactant
The volume ratio of temperature -60 is 3.5:2:1) it, stirs, heat temperature to 155 DEG C, boiling 2.5h, cooling, filtering, the filter residue of collection is with having
After solvent is rinsed repeatedly, then rinsed with deionized water；
(3) soda boiling is handled：Filter residue is added into the filter residue rinsed by organic solvent flushing, deionized water in step (2)
The mixed liquor of the lye-organic solvent of 12 times of volumes of weight be (0.8mol sodium hydroxide solutions/potassium hydroxide solution-isopropanol
Mixed liquor, and the volume ratio 3 of lye and isopropanol:1), heating temperature is to 115 DEG C, under conditions of the power of ultrasonic wave is 365w,
It is ultrasonically treated 3h, is again heated to 145 DEG C of boiling 2.5h, is filtered, solid-state filtrate is collected；
(4) bleaching：Solid-state filtrate in step (3) is taken, the organic acid-of solid-state filtrate 10 times of volumes of weight is added
Bleaching agent (mixed liquor of acetic acid-sodium sulfite) mixed liquor, most 95 DEG C of heating temperature bleach 1.8h, obtain false indigo and starch in vain；
(5) microwave treatment：False indigo in step (4) is taken to starch in vain, according to volume ratio 1:It is molten that calcium hydroxide is added in 6 ratio
Liquid is 260w in power, and temperature is handled under conditions of being 115 DEG C, filtered, and drying obtains false indigo cellulose.
The yield of false indigo cellulose is 84.18% under this process condition.
Example 4
A method of cellulose being extracted using the false indigo of salt-soda soil plantation, is included the following steps：
(1) it pre-processes：By false indigo peeling, crushing, sieving, drying, cooling, false indigo wood powder is obtained；
(2) Acid treatment：False indigo wood powder in step (1) is taken, the organic molten of false indigo wood powder 15 times of volumes of weight is added
(volumetric concentration is the mixed liquor of 80% ethyl alcohol-tartaric acid-Tween-60, and second to the mixed liquor of agent-organic acid-surfactant
The volume ratio of alcohol, tartaric acid and Tween-60 is 5:3:2) it, stirs, heat temperature to 180 DEG C, boiling 3h, cooling is filtered, collection
After filter residue is rinsed repeatedly with organic solvent, then rinsed with deionized water；
(3) soda boiling is handled：Filter residue is added into the filter residue rinsed by organic solvent flushing, deionized water in step (2)
Lye-the organic solvent of 15 times of volumes of weight mixed liquor (mixed liquor of 1mol sodium hydroxide solutions-isopropanol, and lye with
The volume ratio 3.5 of isopropanol:1), heating temperature is to 120 DEG C, under conditions of the power of ultrasonic wave is 400w, is ultrasonically treated 4h, then
150 DEG C of boiling 3h are heated to, are filtered, solid-state filtrate is collected；
(4) bleaching：Solid-state filtrate in step (3) is taken, the organic acid-of solid-state filtrate 12 times of volumes of weight is added
Bleaching agent (mixed liquor of acetic acid-sodium sulfite) mixed liquor, most 100 DEG C of heating temperature bleach 2h, obtain false indigo and starch in vain；
(5) microwave treatment：False indigo in step (4) is taken to starch in vain, according to volume ratio 1:It is molten that calcium hydroxide is added in 8 ratio
Liquid is 300w in power, and temperature is handled under conditions of being 120 DEG C, filtered, and drying obtains false indigo cellulose.
The yield of false indigo cellulose is 83.25% under this process condition.
In order to preferably prove the preparation method using the present invention obtaining for cellulose products can be improved to extract cellulose
Rate, the present invention have done 3 comparative examples simultaneously.
Comparative example 1
As different from Example 3, step (2) addition is the mixed liquor of ethyl alcohol and tartaric acid, remaining condition is identical, this
The yield of false indigo cellulose is 77.68% under process conditions.
Comparative example 2
As different from Example 3, step (3) addition is ethyl alcohol and acid, is not ultrasonically treated, remaining condition phase
Together, the yield of false indigo cellulose is 77.85% under this process conditions.
Comparative example 3
As different from Example 3, bleaching agent is only added in step (4), and without carrying out microwave treatment in step (5),
Remaining condition is identical, and the yield of false indigo cellulose is 78.42% under this process conditions.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (10)
1. a kind of method that false indigo using salt-soda soil plantation extracts cellulose, it is characterised in that the method includes following steps
Suddenly：
(1) it pre-processes：By false indigo peeling, crushing, sieving, drying, cooling, false indigo wood powder is obtained；
(2) Acid treatment：False indigo wood powder in step (1) is taken, the mixed liquor of organic solvent-organic acid-surfactant is added,
Stirring, heating boiling, cooling, filtering after the filter residue of collection is rinsed repeatedly with organic solvent, then are rinsed with deionized water；
(3) soda boiling is handled：It is organic to being rinsed by organic solvent in step (2), lye-being added in the filter residue that deionized water is rinsed
The mixed liquor of solvent heats boiling, solid-state filtrate is collected in filtering by being ultrasonically treated；
(4) bleaching：Solid-state filtrate in step (3) is taken, organic acid-bleaching agent mixed liquor is added and is bleached, purple is obtained
Fringe Chinese scholartree is starched in vain；
(5) microwave treatment：It takes false indigo in step (4) to starch addition calcium hydroxide solution in vain, is filtered after microwave treatment, drying obtains
False indigo cellulose.
2. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 extracts cellulose, feature exist
In：Organic solvent is ethyl alcohol, n-butanol or isopropyl in the mixed liquor of organic solvent-organic acid-surfactant in step (2)
Alcohol；Organic acid is citric acid, tartaric acid or oxalic acid；Surfactant is neopelex or Tween-60.
3. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 extracts cellulose, feature exist
In：The mixed liquor of the organic solvent-organic acid-surfactant is the mixing of ethyl alcohol/isopropanol-tartaric acid-Tween-60
Liquid.
4. the method that a kind of false indigo using salt-soda soil plantation according to claim 3 extracts cellulose, feature exist
In：The volumetric concentration of the ethyl alcohol is 65%-80%.
5. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 extracts cellulose, feature exist
In：The temperature of boiling is 120-180 DEG C in step (2), and the time of boiling is 1-3h.
6. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 extracts cellulose, feature exist
In：Temperature when step (3) is ultrasonically treated is 80-120 DEG C, time 1-4h, and the power of ultrasonic wave is 200-400w.
7. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 extracts cellulose, feature exist
In：The mixed liquor of lye-organic solvent in step (3) is 0.5-1mol sodium hydroxide solutions/potassium hydroxide solution-isopropanol
Mixed liquor.
8. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 extracts cellulose, feature exist
In：The mixed liquor of organic acid-bleaching agent is the mixing of acetic acid-tetraacetyl ethylene diamine/sodium hypochlorite/sodium sulfite in step (4)
Liquid.
9. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 extracts cellulose, feature exist
In：Bleaching temperature is 60-100 DEG C in step (4), bleaching time 1-2h.
10. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 extracts cellulose, feature exist
In：The power of microwave treatment is 200-300w in step (5), and temperature is 80-120 DEG C.
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| CN201711455090.3A CN108330723B (en) | 2017-12-28 | 2017-12-28 | Method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil |
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| CN201711455090.3A CN108330723B (en) | 2017-12-28 | 2017-12-28 | Method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110130135A (en) * | 2019-05-28 | 2019-08-16 | 西北农林科技大学 | A kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material |
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| US5219601A (en) * | 1991-03-15 | 1993-06-15 | Elf Atochem S.A. | Two-step bleaching of plant materials |
| CN102277760A (en) * | 2011-08-30 | 2011-12-14 | 内蒙古科技大学 | Pre-processing method in process of producing paper pulp |
| CN103669064A (en) * | 2013-12-13 | 2014-03-26 | 四川永丰纸业股份有限公司 | Preparation process of acetified bamboo pulp |
| CN104357931A (en) * | 2014-11-28 | 2015-02-18 | 赵兵 | Fluorescent salix mongolica regenerated cellulose fibers and preparation method thereof |
| 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 |
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2017
- 2017-12-28 CN CN201711455090.3A patent/CN108330723B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5219601A (en) * | 1991-03-15 | 1993-06-15 | Elf Atochem S.A. | Two-step bleaching of plant materials |
| CN102277760A (en) * | 2011-08-30 | 2011-12-14 | 内蒙古科技大学 | Pre-processing method in process of producing paper pulp |
| CN103669064A (en) * | 2013-12-13 | 2014-03-26 | 四川永丰纸业股份有限公司 | Preparation process of acetified bamboo pulp |
| CN104357931A (en) * | 2014-11-28 | 2015-02-18 | 赵兵 | Fluorescent salix mongolica regenerated cellulose fibers and preparation method thereof |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110130135A (en) * | 2019-05-28 | 2019-08-16 | 西北农林科技大学 | A kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material |
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