CN109750547A - A method of nano-cellulose is prepared using sugaring by-product bagasse - Google Patents
A method of nano-cellulose is prepared using sugaring by-product bagasse Download PDFInfo
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- CN109750547A CN109750547A CN201910171545.1A CN201910171545A CN109750547A CN 109750547 A CN109750547 A CN 109750547A CN 201910171545 A CN201910171545 A CN 201910171545A CN 109750547 A CN109750547 A CN 109750547A
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Abstract
The invention discloses a kind of methods for preparing nano-cellulose using sugaring by-product bagasse.The method for utilizing sugaring by-product bagasse to prepare nano-cellulose includes drying, crushing, bleaching delignification fibre, Fine by Ultrasonic and high-pressure homogenization step.The method of the present invention can avoid the influence and harm to ecological environment, eliminate fire safety evaluating hidden danger, improve the added value of bagasse, generate economic, society and ecological benefits rationally efficiently using sugaring by-product bagasse；Using nano-cellulose made from the method for the present invention, 20 ~ 300nm of diameter, large specific surface area has many advantages, such as that mechanical performance height, good biocompatibility, composite reactive are high；Present invention process process is short, easy to operate easy to implement, production cost is low, it is not generated in preparation process to environment harmful side product, product can be dispersed in the multi-solvents such as water, ethyl alcohol, and in the fields such as flexible electronic, functional material, polymer modification, application prospect is wide.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of to prepare nano-cellulose using sugaring by-product bagasse
Method.
Background technique
It is asked based on the macromolecule of fossil resource resource due to caused by its is non-renewable and non-biodegradable and environment
Topic becomes increasingly conspicuous, and sufficiently developing and using renewable resource becomes inexorable trend.Currently, preparing nanofiber using natural biomass
Element replaces the non-renewable resources such as petroleum, metal, is applied to weaving, building materials, automobile, the fields such as personal nursing have become the country
The hot spot of outer research.
Native cellulose is the most abundant biomass resource on the earth, is that most wide boiomacromolecule is distributed in nature,
It is present in various biological such as plants, animal and some bacteriums.Nano-cellulose is diameter less than 100 nm
Super-micro-fine fibres and cellulose minimal physical structural unit, compared with non-nanofiber element, it has high-intensitive, high
The advantages that hydrophily, high transparency, has native cellulose lightweight, degradable, bio-compatible and the characteristics such as renewable in addition,
There is huge potential application foreground in the fields such as papermaking, building, automobile, food, cosmetics, electronic product, medicine.
Bagasse is the by-product of Closed Circulation in Sugar Production, the sugarcane slag ingredient of desiccation include lignin 18 ~ 22%, cellulose 40 ~
50%, hemicellulose 25 ~ 30%, protein 2.5%, coarse ash 2.5%, pectic substance 1.5%, the 1.5-2.5% such as fat, sugar, fiber
Cellulose content is higher than other common natural biomass raw materials.Yunnan Province is the second largest province of cane planting, and sugar industry is that Yunnan Province works as
The pillar project of real estate sector once drove local ethnic group to develop the economy, and realization is shaken off poverty and set out on the road to prosperity, but sucrose produces since nearly more than ten years
Industry is had difficulty in taking a step, and is badly in need of the import of advanced technology and is explored Circular Economy, extension industry chain promotes added value of product, real
Existing sustainable development.Yunnan Province sugarcane year enters squeezing amount at 15,000,000 tons or more, produces about 1,600,000 tons of by-product desiccation bagasse,
Wherein about 1,300,000 tons of supply sugar refinery boilers do fuel, and remaining about 300,000 tons are stacked, and not only pollute environment but also there are fire
Security risk.Prepare nano-cellulose using bagasse, it can be achieved that sugaring by-product bagasse higher value application, have simultaneously
Inexpensively, the advantages such as more, easily collecting, content of cellulose height are measured, are played a significant role to the sugar industry development for pushing Yunnan.At present
The method for preparing nano-cellulose is needed mostly by multistep alkali, acid or enzymatic treatment, and process flow is long, higher cost, limitation
The industrialized production and application of nano-cellulose.Therefore it is very necessary for developing a kind of method that can solve above-mentioned technical problem
's.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing nano-cellulose using sugaring by-product bagasse.
The object of the present invention is achieved like this, the side that nano-cellulose is prepared using sugaring by-product bagasse
Method includes drying, crushing, bleaching delignification fibre, Fine by Ultrasonic and high-pressure homogenization step, is specifically included:
A, sugaring by-product bagasse drying: is dried to obtain material a；
B, it crushes: material a be crushed into 40 meshes and obtain bagasse powder b；
C, bleaching delignification is fine: the compound delignification of SODIUM PERCARBONATE of 40 ~ 80 times of bagasse powder b weight will be added in bagasse powder b
Reagent is stirred to react 1 ~ 3h under the conditions of 30 ~ 70 DEG C of temperature and is bleached, then heats to 80 ~ 120 DEG C and be stirred to react 1 ~ 5h
Except impurity such as lignin and hemicelluloses, filters to take residue washing and drain to neutrality and obtain material c；
D, Fine by Ultrasonic: the deionized water of 40 ~ 120 times of bagasse powder b weight will be added in material c, ultrasonication is touched
Feel the semigel state cellulose d without granular sensation；
E, high-pressure homogeneous: sense of touch is obtained into object nano-cellulose without the semigel state cellulose d homogeneous of granular sensation.
The invention has the following advantages that
1) influence and danger to ecological environment can be avoided rationally efficiently using sugaring by-product bagasse using the method for the present invention
Evil eliminates fire safety evaluating hidden danger, improves the added value of bagasse, generates economic, society and ecological benefits；
2) nano-cellulose made from the method for the present invention, 20 ~ 300nm of diameter, large specific surface area, with mechanical performance are utilized
The advantages that height, good biocompatibility, high composite reactive；
3) it solves the problems, such as that the prior art is difficult to be simple and efficient and prepares nano-cellulose using plant fiber；
4) process flow is short, easy to operate easy to implement, and production cost is low, is not generated in preparation process to environment nocuousness by-product
Object；
5) gained nano-cellulose retains cellulose surface-OH, and introduces without other groups, and product can be dispersed in water, second
The multi-solvents such as alcohol, in the fields such as flexible electronic, functional material, polymer modification, application prospect is wide.
Detailed description of the invention
Fig. 1 is the transmission electron microscope photo of bagasse nano-cellulose prepared by specific embodiment one；
Fig. 2 is the transmission electron microscope photo of bagasse nano-cellulose prepared by specific embodiment two.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is further illustrated, but is not subject in any way to the present invention
Limitation, based on present invention teach that it is made it is any transform or replace, all belong to the scope of protection of the present invention.
The method of the present invention for preparing nano-cellulose using sugaring by-product bagasse includes dry, crushing, drift
Butter fibre, Fine by Ultrasonic and high-pressure homogenization step, specifically include:
A, sugaring by-product bagasse drying: is dried to obtain material a；
B, it crushes: material a be crushed into 40 meshes and obtain bagasse powder b；
C, bleaching delignification is fine: the compound delignification of SODIUM PERCARBONATE of 40 ~ 80 times of bagasse powder b weight will be added in bagasse powder b
Reagent is stirred to react 1 ~ 3h under the conditions of 30 ~ 70 DEG C of temperature and is bleached, then heats to 80 ~ 120 DEG C and be stirred to react 1 ~ 5h
Except impurity such as lignin and hemicelluloses, filters to take residue washing and drain to neutrality and obtain material c；
D, Fine by Ultrasonic: the deionized water of 40 ~ 120 times of bagasse powder b weight will be added in material c, ultrasonication is touched
Feel the semigel state cellulose d without granular sensation；
E, high-pressure homogeneous: sense of touch is obtained into object nano-cellulose without the semigel state cellulose d homogeneous of granular sensation.
Drying described in step A is drying or air-dries.
The temperature of the drying is 40 ~ 50 DEG C.
Crushing described in step B is to be mechanically pulverized.
The crushing is that the pulverizer that material a revolving speed is 3000 ~ 10000r/min is handled 30 ~ 60s.
The composition and mass volume ratio concentration of the compound delignification reagent of SODIUM PERCARBONATE described in step C are as follows: 4 ~ 10%
2Na2CO3·3H2O2、0.5~2.0% Na3PO4、0.5~2.0% Na2SiO3With 2 ~ 6% NaOH.
Ultrasonication described in D step be under 15 ~ 35 DEG C of temperature, power 600W conditions above ultrasonication 30 ~
90min。
Homogeneous described in E step is that homogeneous is carried out under the conditions of different pressures, specifically: successively press 10MPa 1 ~ 3 time,
30MPa 2 ~ 4 times, 60MPa 3 ~ 5 times, 4 ~ 6 progress homogeneous of 100MPa obtain object nano-cellulose.
The homogeneous specifically: successively press 10Mpa 1 ~ 3 time, homogenizing time is every time 40 ~ 60min；30MPa 2~4
Secondary, homogenizing time is every time 30 ~ 50min；60MPa 3 ~ 5 times, homogenizing time is every time 20 ~ 40min；100MPa 4 ~ 6 times,
The matter time is every time 10 ~ 30min, finally obtains object nano-cellulose.
The diameter of the object cellulose is 20 ~ 300nm, draw ratio a height of 20 ~ 50.
Case is embodied, the present invention will be further described below:
Embodiment 1
(1) acquisition sampling drying: is dried into (or air-drying) from 45 DEG C of bagasse of Yunnan sugar refinery Dehong Jing Han bagasse library；(2) machine
Tool crushes: the high speed disintegrator of the bagasse raw material after drying handled into 30 s, crosses 40 mesh screens, the fibre after weighing 6 g sieving
Tie up powder；(3) bleaching delignification is fine: weighed bagasse powder being transferred to three-necked flask, the compound de- wood of 200 g SODIUM PERCARBONATEs is added
Plain reagent (2Na2CO3·3H2O2/Na3PO4·12H2O/Na2SiO3·9H2The mass volume ratio of O/NaOH/ water is 6.0/0.8/
0.8/2/100) 60 min, are stirred to react at 60 DEG C, is decomposed using SODIUM PERCARBONATE and generates hydrogen peroxide bleaching, be then warming up to
90 DEG C, the 3 h removal impurity such as lignin and hemicellulose are stirred to react, residue washing is filtered to take and drains to neutrality；(4) ultrasonic
Refinement: the filter residue that filtering and washing is obtained is added in 300 g deionized waters, at a temperature of 20 DEG C of constant temperature, keeps 600W or more
Power, be spaced 3 s, through ultrasonic cell disintegration instrument be crushed 80 min, obtain semigel state cellulose of the sense of touch without granular sensation；
(5) high-pressure homogeneous: the semigel state cellulose that will be obtained under the conditions of different pressures homogeneous several times, specifically: 10MPa 1 time,
30MPa 2 times, 60MPa 3 times, 100MPa 4 times, obtaining the slightly bluish nano-grade cellulosic of color later, diameter is 20 ~
300nm, draw ratio a height of 20 ~ 50.
The transmission electron microscope photo of the bagasse nano-cellulose of present embodiment preparation is as shown in Figure 1, can from figure
To find out, bagasse nano-cellulose diameter is 20 ~ 300nm, and length is in several microns.
Embodiment 2
(1) acquisition sampling drying: is dried into (or air-drying) from 45 DEG C of bagasse of Yunnan Dehong Ruili sugar refinery bagasse library；(2) machine
Tool crushes: the high speed disintegrator of the bagasse raw material after drying handled into 60 s, crosses 40 mesh screens, the fibre after weighing 6 g sieving
Tie up powder；(3) bleaching delignification is fine: weighed bagasse powder being transferred to three-necked flask, the compound de- wood of 400 g SODIUM PERCARBONATEs is added
Plain reagent (2Na2CO3·3H2O2/Na3PO4·12H2O/Na2SiO3·9H2The mass volume ratio of O/NaOH/ water is 9.0/1.6/
1.6/4/100) 1.5 h, are stirred to react at 50 DEG C, is decomposed using SODIUM PERCARBONATE and generates hydrogen peroxide bleaching, be then warming up to
80 DEG C, the 4 h removal impurity such as lignin and hemicellulose are stirred to react, residue washing is filtered to take and drains to neutrality；(4) ultrasonic
Refinement: the filter residue that filtering and washing is obtained is added in 500 g deionized waters, at a temperature of 20 DEG C of constant temperature, keeps 600W or more
Power, be spaced 3 s, through ultrasonic cell disintegration instrument be crushed 60 min, obtain semigel state cellulose of the sense of touch without granular sensation；
(5) high-pressure homogeneous: the semigel state cellulose that will be obtained under the conditions of different pressures homogeneous several times, specifically: 10MPa 2 times,
30MPa 2 times, 60MPa 3 times, 100MPa 4 times, obtaining the slightly bluish nano-grade cellulosic of color later, diameter is 20 ~
300nm, draw ratio a height of 20 ~ 50.
The transmission electron microscope photo of the bagasse nano-cellulose of present embodiment preparation is as shown in Fig. 2, can from figure
To find out, bagasse nano-cellulose diameter is 20 ~ 300nm, and length is in several microns.
Claims (10)
1. a kind of method for preparing nano-cellulose using sugaring by-product bagasse, it is characterised in that described is secondary using sugaring
The method that product bagasse prepares nano-cellulose includes dry, crushing, bleaching delignification fibre, Fine by Ultrasonic and high-pressure homogenization step,
It specifically includes:
A, sugaring by-product bagasse drying: is dried to obtain material a；
B, it crushes: material a be crushed into 40 meshes and obtain bagasse powder b；
C, bleaching delignification is fine: the compound delignification of SODIUM PERCARBONATE of 40 ~ 80 times of bagasse powder b weight will be added in bagasse powder b
Reagent is stirred to react 1 ~ 3h under the conditions of 30 ~ 70 DEG C of temperature and is bleached, then heats to 80 ~ 120 DEG C and be stirred to react 1 ~ 5h
Except lignin and hemicellulose impurities, filters to take residue washing and drain to neutrality and obtain material c；
D, Fine by Ultrasonic: the deionized water of 40 ~ 120 times of bagasse powder b weight will be added in material c, ultrasonication is touched
Feel the semigel state cellulose d without granular sensation；
E, high-pressure homogeneous: sense of touch is obtained into object nano-cellulose without the semigel state cellulose d homogeneous of granular sensation.
2. the method according to claim 1 for preparing nano-cellulose using sugaring by-product bagasse, it is characterised in that A
Drying described in step is drying or air-dries.
3. the method according to claim 2 for preparing nano-cellulose using sugaring by-product bagasse, it is characterised in that
The temperature of the drying is 40 ~ 50 DEG C.
4. the method according to claim 1 for preparing nano-cellulose using sugaring by-product bagasse, it is characterised in that B
Crushing described in step is to be mechanically pulverized.
5. the method according to claim 1 or 4 for preparing nano-cellulose using sugaring by-product bagasse, feature exist
It is that the pulverizer that material a revolving speed is 3000 ~ 10000r/min is handled into 30 ~ 60s in the crushing.
6. the method according to claim 1 for preparing nano-cellulose using sugaring by-product bagasse, it is characterised in that C
The composition and mass volume ratio concentration of the compound delignification reagent of SODIUM PERCARBONATE described in step are as follows: 4 ~ 10% 2Na2CO3·
3H2O2、0.5~2.0% Na3PO4、0.5~2.0% Na2SiO3With 2 ~ 6% NaOH.
7. the method according to claim 1 for preparing nano-cellulose using sugaring by-product bagasse, it is characterised in that D
Ultrasonication described in step is 30 ~ 90min of ultrasonication under 15 ~ 35 DEG C of temperature, power 600W conditions above.
8. the method according to claim 1 for preparing nano-cellulose using sugaring by-product bagasse, it is characterised in that E
Homogeneous described in step is that homogeneous is carried out under the conditions of different pressures, specifically: it successively presses 10MPa 1 ~ 3 time, 30MPa 2 ~ 4
Secondary, 60MPa 3 ~ 5 times, 4 ~ 6 progress homogeneous of 100MPa obtain object nano-cellulose.
9. the method for preparing nano-cellulose using sugaring by-product bagasse according to claim 1 or 8, feature exist
In the homogeneous specifically: successively press 10Mpa 1 ~ 3 time, homogenizing time is every time 5 ~ 20min；30MPa 2 ~ 4 times, homogeneous
Time is every time 5 ~ 15min；60MPa 3 ~ 5 times, homogenizing time is every time 5 ~ 10min；100MPa 4 ~ 6 times, homogenizing time is every
Secondary 5 ~ 10min finally obtains object nano-cellulose.
10. the method according to claim 1 for preparing nano-cellulose using sugaring by-product bagasse, it is characterised in that
The diameter of the object cellulose is 20 ~ 300nm, draw ratio a height of 20 ~ 50.
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| CN111850070A (en) * | 2020-07-28 | 2020-10-30 | 暨南大学 | Method for pretreating bagasse by using sodium phosphate and hydrogen peroxide |
| RU2768635C1 (en) * | 2021-07-16 | 2022-03-24 | Публичное акционерное общество «Татнефть» имени В.Д. Шашина | Method for obtaining flaxseed pulp |
| CN114231569A (en) * | 2021-12-23 | 2022-03-25 | 清华大学 | Method for preparing ethanol and co-producing cellulose nanofibers through alkali distillation |
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