CN110373441A - A kind of preparation method of high length-diameter ratio nano-cellulose - Google Patents
A kind of preparation method of high length-diameter ratio nano-cellulose Download PDFInfo
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- CN110373441A CN110373441A CN201910495037.9A CN201910495037A CN110373441A CN 110373441 A CN110373441 A CN 110373441A CN 201910495037 A CN201910495037 A CN 201910495037A CN 110373441 A CN110373441 A CN 110373441A
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 53
- 239000001913 cellulose Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000002002 slurry Substances 0.000 claims abstract description 24
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 238000010009 beating Methods 0.000 claims abstract description 10
- 239000000084 colloidal system Substances 0.000 claims abstract description 9
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 6
- 239000011707 mineral Substances 0.000 claims abstract description 6
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 230000002255 enzymatic effect Effects 0.000 claims abstract description 4
- 108090000790 Enzymes Proteins 0.000 claims description 18
- 102000004190 Enzymes Human genes 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 108010059892 Cellulase Proteins 0.000 claims description 10
- 229920002522 Wood fibre Polymers 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 101710112457 Exoglucanase Proteins 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011121 hardwood Substances 0.000 claims description 6
- 239000011122 softwood Substances 0.000 claims description 6
- 108010047754 beta-Glucosidase Proteins 0.000 claims description 5
- 102000006995 beta-Glucosidase Human genes 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 3
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 3
- 241001330002 Bambuseae Species 0.000 claims description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 239000011425 bamboo Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 229940088598 enzyme Drugs 0.000 description 16
- 238000000227 grinding Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 229920001503 Glucan Polymers 0.000 description 3
- 238000011953 bioanalysis Methods 0.000 description 3
- 238000009955 starching Methods 0.000 description 3
- 235000010215 titanium dioxide Nutrition 0.000 description 3
- 238000005903 acid hydrolysis reaction Methods 0.000 description 2
- 229940106157 cellulase Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 241001343274 Dichrostachys spicata Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 108010089934 carbohydrase Proteins 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- -1 floor Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000008104 plant cellulose Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
-
- 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
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
- D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/02—Methods of beating; Beaters of the Hollander type
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Biochemistry (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biotechnology (AREA)
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- Genetics & Genomics (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention provides a kind of preparation methods of high length-diameter ratio nano-cellulose, this method is by lignocellulosic through compound bio enzymatic treatment, and lignocellulosic is beaten with beater to certain beating degree by treated, obtained slurry carries out colloid mill circular treatment after adding suitable dispersing agent or ground minerals, and with the increase of cycle-index, abrasive disk space is constantly reduced, high length-diameter ratio nano-cellulose is obtained.The present invention overcomes prepare the agglomeration traits that energy consumption needed for nano-cellulose is high and high length-diameter ratio nano-cellulose occurs by hydrogen bond action during the preparation process.
Description
Technical field
The present invention relates to a kind of preparation methods of high length-diameter ratio nano-cellulose, belong to Bio-Nano-Materials field.
Background technique
With the continuous social and economic development, the problems such as non-renewable resources are increasingly deficient, environmental pollution becomes increasingly conspicuous, wood
Material fiber as renewable resource abundant on the earth, the fields such as science, medicine, the energy, health application increasingly by
Pay attention to.Nano-cellulose is that have 1-dimention nano ruler by chemistry, physics or bioanalysis preparation using fibrous material as raw material
Very little cellulose derivative materials, it is because of its biodegradable, bio-compatible, large specific surface area, and good mechanical performance etc. is all
More good characteristics can be used for the fields such as medicine, packaging, papermaking, food additives, paint, floor, building materials.
As a kind of emerging Bio-Nano-Materials, nano-cellulose receives the extensive concern of all circles.Preparation method
It is divided into chemical method, physical method and bioanalysis etc..It includes mineral acid hydrolysis method and cellulase water that chemical method, which prepares nano-cellulose,
Solution.Mineral acid hydrolysis method realizes the hydrolysis of cellulose using strong acid, improves product by using modes such as ultrasound pretreatments and obtains
Rate shortens the reaction time；Temperature, reaction time, the type of strong acid and concentration, the dosage of plant cellulose in hydrolytic process etc.
It will affect the property of nano-cellulose, which can generate a large amount of spent acid and impurity, a large amount of water and power resource are consumed, and
Consersion unit is required high, it is desirable that equipment is resistant to strong acid, in addition carries out recycling to the residue after reaction and processing is compared
It is difficult.Cellulose hydrolyzation method removes cellulose amorphous region using the stronger cellulase of selectivity, is left cellulose knot
Crystalline region, the method process conditions are mild, and specificity is strong.Physical method refers to through pressure, friction, the physical means such as heating explosion, real
The separation of existing cellulose is decomposed, and nano-grade cellulosic is prepared.Its simple process, it is easily operated, but need using special
Equipment, energy consumption is relatively high, and the nano-cellulose particle diameter distribution of preparation is wide, is in addition also easy to occur homogenizer blocking etc. and asks
Topic, cannot achieve preparation process serialization.Bioanalysis prepares that nano-cellulose is complicated for operation, and time-consuming, at high cost, although domestic
Outer research is more, but is not used widely.Therefore research and development goes out novel simple, green, low energy consumption, efficient preparation
Nano-cellulose method is very urgent.
Summary of the invention
The purpose of the present invention is to provide a kind of high length-diameter ratios that a kind of low energy consumption and effectively solution nano-cellulose are reunited
The preparation method of nano-cellulose.
The technical solution adopted by the present invention is that: a kind of preparation method of high length-diameter ratio nano-cellulose, it is characterised in that its
Preparation process is by certain density wood fibre at 25~50 DEG C, pH be 6.5~8.5 under conditions of through compound bio enzymatic treatment
The obtained slurry of processing, is diluted with water to after the concentration of 1.5~2.5w% that be beaten with beater to beating degree be 65 by 12~48h
~95 ° of SR, obtained slurry press the dispersing agent or ground of oven dry weight addition 0.1~1w ‰ relative to wood fibre
Particle diameter carry out colloid mill circular treatment after the minerals of 10~200nm, cycle-index is 2~10 times, and with following
The increase of ring number, constantly reduction abrasive disk space, obtain the high length-diameter ratio nano-cellulose that draw ratio is 500~2000.
The preparation method of a kind of high length-diameter ratio nano-cellulose, it is characterised in that lignocellulosic is needlebush
One or more of slurry, hardwood pulp or bamboo pulp.
The preparation method of a kind of high length-diameter ratio nano-cellulose, it is characterised in that the concentration of lignocellulosic is 2
~5%.
The preparation method of a kind of high length-diameter ratio nano-cellulose, it is characterised in that compound biological enzyme is poly- for inscribe Portugal
Carbohydrase, exoglucanase and beta-glucosidase are compounded according to the ratio of 10~30 ︰, 5~20 ︰ 1~5.
The preparation method of a kind of high length-diameter ratio nano-cellulose, it is characterised in that the additive amount of compound biological enzyme is pressed
Oven dry weight relative to wood fibre is 50~150ppm.
The preparation method of a kind of high length-diameter ratio nano-cellulose, it is characterised in that dispersing agent is polyethylene glycol oxide
PEO or polyacrylamide PAM.
The preparation method of a kind of high length-diameter ratio nano-cellulose, it is characterised in that minerals are talcum powder, kaolinite
The mixture of one or more of native or titanium dioxide.
Using the present invention, energy consumption can be effectively reduced by compound enzymatic treatment, and solve to receive in mashing and process of lapping
Rice cellulose agglomeration traits, and preparation method is environmentally protective.
Specific embodiment
The present invention is explained in further detail below with reference to embodiment, but embodiment of the present invention is without being limited thereto.
One, embodiment one.
The high length-diameter ratio nano-cellulose the preparation method is as follows: weigh 1000g softwood pulp, it is 2% that it is dense, which to add water to slurry,
At 25 DEG C, the compound biological enzyme through 150ppm is (by endoglucanase, exoglucanase and β-Portugal under conditions of pH is 6.5
Polyglycoside enzyme is compounded in 10 ︰, 5 ︰, 1 ratio) processing 12h, is used treated after slurry is diluted with water to the concentration of 1.5w%
It is 65 ° of SR that watt power beater, which is beaten to beating degree, and obtained slurry adds ‰ polyethylene glycol oxide of 0.1w, after mixing evenly,
Carry out circular treatment in colloid mill, every circulation reduces an abrasive disk space twice, circular grinding 2 times, obtain draw ratio be 500~
1000 nano-cellulose.
Two, embodiment two.
The high length-diameter ratio nano-cellulose the preparation method is as follows: weigh 1000g softwood pulp, it is 3% that it is dense, which to add water to slurry,
At 30 DEG C, the compound biological enzyme through 100ppm is (by endoglucanase, exoglucanase and β-Portugal under conditions of pH is 7.5
Polyglycoside enzyme is compounded in 15 ︰, 10 ︰, 5 ratio) processing for 24 hours, by after treated slurry the is diluted with water to concentration of 2w% with watt
It is 75 ° of SR that power beater, which is beaten to beating degree, and obtained slurry adds ‰ polyacrylamide of 0.5w, after mixing evenly, in glue
Carry out circular treatment in body mill, every circulation reduces an abrasive disk space twice, circular grinding 4 times, obtain draw ratio be 800~
1200 nano-cellulose.
Three, embodiment three.
The high length-diameter ratio nano-cellulose the preparation method is as follows: weigh each 500g of softwood pulp, hardwood pulp, add water to
Starching dense is 4%, and at 40 DEG C, the compound biological enzyme through 50ppm is (by endoglucanase, circumscribed glucan under conditions of pH is 6.5
Enzyme and beta-glucosidase are compounded in the ratio of 30 ︰, 20 ︰ 5) processing 48h, by treated, slurry is diluted with water to 2.5w%
Concentration after to be beaten with a watt power beater to beating degree be 85 ° of SR, obtained slurry adds ‰ polyethylene glycol oxide of 0.5w, stirring
After uniformly, circular treatment is carried out in colloid mill, every circulation reduces an abrasive disk space twice, circular grinding 6 times, obtains major diameter
Than the nano-cellulose for 800~1500.
Four, example IV.
The high length-diameter ratio nano-cellulose the preparation method is as follows: weigh each 500g of softwood pulp, hardwood pulp, add water to
Starching dense is 5%, and at 50 DEG C, the compound biological enzyme through 100ppm is (by endoglucanase, circumscribed glucan under conditions of pH is 8.5
Enzyme and beta-glucosidase are compounded in 15 ︰, 10 ︰, 3 ratio) processing 48h, by treated, slurry is diluted with water to 1.5w%'s
Being beaten with a watt power beater to beating degree after concentration is 95 ° of SR, obtained slurry addition 0.1w ‰ ground particle diameter
In the talcum powder of 10-200nm, after mixing evenly, circular treatment is carried out in colloid mill, every circulation reduces twice between a mill
Gap circular grinding 8 times, obtains the nano-cellulose that draw ratio is 1000~2000.
Five, embodiment five.
The high length-diameter ratio nano-cellulose the preparation method is as follows: weigh each 500g of softwood pulp, hardwood pulp, add water to
Starching dense is 5%, and at 50 DEG C, the compound biological enzyme through 150ppm is (by endoglucanase, circumscribed glucan under conditions of pH is 8.5
Enzyme and beta-glucosidase are compounded in 10 ︰, 15 ︰, 1 ratio) processing 48h, by treated, slurry is diluted with water to the dense of 2w%
Being beaten with a watt power beater to beating degree after degree is 95 ° of SR, and obtained slurry addition 0.5w ‰ ground particle diameter exists
The kaolin of 10~200nm carries out circular treatment after mixing evenly in colloid mill, and every circulation reduces twice between a mill
Gap circular grinding 10 times, obtains the nano-cellulose that draw ratio is 1200~2000.
Six, embodiment six.
The high length-diameter ratio nano-cellulose the preparation method is as follows: weigh hardwood pulp 1000g, it is 5% that it is dense, which to add water to slurry,
At 50 DEG C, the compound biological enzyme through 100ppm is (by endoglucanase, exoglucanase and β-Portugal under conditions of pH is 8.5
Polyglycoside enzyme is compounded in 15 ︰, 15 ︰, 2 ratio) processing 48h, is used treated after slurry is diluted with water to the concentration of 2.5w%
It is 95 ° of SR that watt power beater, which is beaten to beating degree, and obtained slurry addition 1w ‰ ground particle diameter is in 10~200nm
Talcum powder and titanium white powder mixture carry out circular treatment in colloid mill after mixing evenly, every circulation reduces primary mill twice
Dish gap circular grinding 10 times, obtains the nano-cellulose that draw ratio is 1200~2000.
Seven, embodiment seven.
The high length-diameter ratio nano-cellulose the preparation method is as follows: weigh bamboo pulp 1000g, it is 5% that it is dense, which to add water to slurry, 50
DEG C, the compound biological enzyme through 150ppm is (by endoglucanase, exoglucanase and β-glucose under conditions of pH is 7.0
Glycosides enzyme is compounded in 25 ︰, 15 ︰, 5 ratio) processing 48h, by after treated slurry the is diluted with water to concentration of 2.5w% with watt power
It is 95 ° of SR that beater, which is beaten to beating degree, cunning of the obtained slurry addition 1w ‰ ground particle diameter in 10~200nm
Mountain flour, kaolin and titanium white powder mixture carry out circular treatment after mixing evenly in colloid mill, and every circulation reduces one twice
Secondary abrasive disk space, circular grinding 10 times, obtaining draw ratio is 800~1500 nano-celluloses.
Claims (7)
1. a kind of preparation method of high length-diameter ratio nano-cellulose, it is characterised in that its preparation process is will be certain density wooden
Fiber at 25~50 DEG C, pH be 6.5~8.5 under conditions of through compound bio 12~48h of enzymatic treatment, slurry that processing obtains is added
It is 65~95 ° of SR that water, which is diluted to after the concentration of 1.5~2.5w% and is beaten with beater to beating degree, and obtained slurry is by opposite
In wood fibre oven dry weight addition 0.1~1w ‰ dispersing agent or ground particle diameter 10~200nm mine
Colloid mill circular treatment is carried out after substance, cycle-index is 2~10 times, and with the increase of cycle-index, constantly reduction mill
Gap obtains the high length-diameter ratio nano-cellulose that draw ratio is 500~2000.
2. a kind of preparation method of high length-diameter ratio nano-cellulose according to claim 1, it is characterised in that wood fibre
Element is one or more of softwood pulp, hardwood pulp or bamboo pulp.
3. a kind of preparation method of high length-diameter ratio nano-cellulose according to claim 1, it is characterised in that wood fibre
The concentration of element is 2~5%.
4. a kind of preparation method of high length-diameter ratio nano-cellulose according to claim 1, it is characterised in that compound bio
Enzyme be endoglucanase, exoglucanase and beta-glucosidase according to 10~30 ︰, 5~20 ︰ 1~5 ratio compounding and
At.
5. a kind of preparation method of high length-diameter ratio nano-cellulose according to claim 1, it is characterised in that compound bio
It is 50~150ppm that the additive amount of enzyme, which is pressed relative to the oven dry weight of wood fibre,.
6. a kind of preparation method of high length-diameter ratio nano-cellulose according to claim 1, it is characterised in that dispersing agent is
Polyethylene glycol oxide PEO or polyacrylamide PAM.
7. a kind of preparation method of high length-diameter ratio nano-cellulose according to claim 1, it is characterised in that minerals are
The mixture of one or more of talcum powder, kaolin or titanium dioxide.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114481675A (en) * | 2021-12-21 | 2022-05-13 | 浙江金昌特种纸股份有限公司 | Method for preparing cellulose microfibril film from wheat straws |
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