CN107345372B - A method of it is prepared based on biomass material cellulose nano-fibrous - Google Patents
A method of it is prepared based on biomass material cellulose nano-fibrous Download PDFInfo
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- CN107345372B CN107345372B CN201610290757.8A CN201610290757A CN107345372B CN 107345372 B CN107345372 B CN 107345372B CN 201610290757 A CN201610290757 A CN 201610290757A CN 107345372 B CN107345372 B CN 107345372B
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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
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/35—Heterocyclic compounds
- D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/507—Polyesters
- D06M15/513—Polycarbonates
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/02—Pretreatment of the raw materials by chemical or physical means
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/12—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by wet methods, by the use of steam
- D21B1/30—Defibrating by other means
- D21B1/36—Explosive disintegration by sudden pressure reduction
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Abstract
Cellulose nano-fibrous method is prepared based on biomass material the present invention discloses a kind of, it include: that biomass material is dried and micronization processes, then by the biological material of generation and organic acid solvent Hybrid Heating reflux separating biomass cellulose, the biomass cellulose isolated is subjected to nanofiber processing using physical method again, obtains the cellulose nano-fibrous of high-purity high length-diameter ratio.The present invention effectively improves the efficiency of preparation, can prepare the cellulose nano-fibrous of high-purity high length-diameter ratio, and reduces the generation of chemical contamination waste, while avoiding in conventional purification methods a series of environmental problems caused by the use of chlorine.
Description
Technical field
The present invention relates to cellulose nano-fibrous preparation methods, more particularly to prepare cellulose as raw material using biomass and receive
The method of rice fiber.
Background technique
Cellulose is the most abundant natural polymer of reserves in the world, by being mechanically pulverized, acid processing or enzyme
Cellulose nano-fibrous (CNF, Cellulose Nanofiber) can be obtained in the processing such as hydrolysis.Cellulose nano-fibrous is a kind of
Superfine fibre, the diameter of every fiber are only 3~4nm, are about as much as two a ten thousandths of hairline.It is cellulose nano-fibrous
With many excellent performances, such as its degree of polymerization is high, crystallinity is high, Young's modulus is high and hardness height, is enhancing it
It is applied in polymer nanocomposites field；Its degradable, good hydrophilic property, the transparency, light weight and good biology
The advantages that compatibility, makes it present good answer in the materials such as artificial creature's tissue, biosensor, flexible electronic device
Use prospect；A large amount of hydroxyl is contained on its surface, its surface is made to be easy to carry out chemical modification, thus assign surface different characteristics,
Further expand its application range.Very tough material can be made using CNF.Compared with steel, the weight of this material
Amount only its 1/5, intensity is its 5 times or more, it for improve Molecularly Imprinted Polymer, composite functional material, high electric mechanical with
And automobile component intensity and realize that equipment lightweight is undoubtedly a kind of excellent selection.
The method of cellulose nanosizing mainly there are into strong acid hydrolysis method, high-strength mechanical method and enzyme hydrolysis method etc. at present.Its
In, the product that strong acid hydrolysis method obtains is corynebacterium nanocrystal, and these types of method can only all handle paper making pulp or warp
The cellulose paste etc. isolated and purified is crossed, and not to from a wealth of sources, content of cellulose natural biomass resource abundant
It is applicable in.
Prepare using biomass material it is cellulose nano-fibrous, first have to carry out the cellulose in biomass separation with
Purifying.Existing processing method mainly separates the cellulose in biomass using acid-hydrolyzed method, then with acid
The sodium chlorite solution of change carries out bleaching to it.And acid waste liquid caused by this separation method is difficult to recycle, it is useless containing chlorine
Liquid is also harmful to ecological environment security；Meanwhile the purity of isolated cellulose in this way is not also highly desirable.Therefore, it visits
Rope it is a kind of to more environment-friendly and high-purity isolation and purification method be prepared using biomass as raw material it is cellulose nano-fibrous
Major issue.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of prepared based on biomass material it is cellulose nano-fibrous
Method can obtain environmentally friendly and high-purity high length-diameter ratio cellulose Nanowire in the preparation using biomass as raw material
Dimension.
In order to solve the above-mentioned technical problems, the present invention provides one kind based on biomass material prepare it is cellulose nano-fibrous
Method, comprising: biomass material is dried and micronization processes, then by the biological material of generation and organic acid solvent
Hybrid Heating reflux separating biomass cellulose, then the biomass cellulose isolated is subjected to nanofiber using physical method
Change processing, obtains the cellulose nano-fibrous of high-purity high length-diameter ratio.
Preferably, by the biological material of generation and organic acid solvent Hybrid Heating reflux separating biomass cellulose, tool
Body include: by biological material and one of aqueous formic acid or arboxylic acid water mixed solution reagent with 1: 5~1: 70 into
Row mixing, wherein the volume content of formic acid is 5~95%, and the volume content of acetic acid is 0~95%, the volume content of water is 5~
80%.
Preferably, dry and refinement includes: to air-dry biomass material in its natural state or in 30~65 DEG C of conditions
Then lower drying will air-dry or the biomass material of drying pulverize and sieve to obtain powdered biological material；Or use physics
Method will air-dry or the biomass material of drying is rubbed into velvet-like biological material.
Preferably, biomass material is dried and micronization processes after and by the biological material of generation with it is organic
Sour solvent Hybrid Heating flows back before separating biomass cellulose, further includes carrying out steam blasting to biological material to pre-process it
Step, it may be assumed that by through pulverizing and sieving generation powdered 10~5000g of biological material or by rubbing at the velvet-like of generation
10~5000g of biological material is packed into reaction vessel, and steam blasting is carried out under 0.5~10.0MPa pressure condition, then will
The hydrolyzate that generates in product centrifuge separation removal blasting process after explosion, and after being separated with distilled water and removing hydrolyzate
Product is washed to neutrality, then washing to neutral product is carried out freeze-drying or supercritical drying processing, is obtained containing biology
The biological material of matter cellulose.
It preferably, further include with hydrogenperoxide steam generator to the biology in biological material before nanofiberization processing
Matter cellulose carries out purification process.
It preferably, further include at being modified cellulose nano-fibrous progress surface after carrying out nanofiber processing
Reason.
Preferably, one of nanofiber processing, including following method are carried out using physical method: using high-pressure homogeneous micro-
Jetting method, or ultrasonic method is used, or use rotary cutting circular grinding method, or use high-speed homogenization method.
Preferably, surface modification treatment includes one of following methods or a variety of: using absorption surface activating agent or poly-
Electrolyte, esterification, etherificate, oxidation, silanization and graft copolymerization, to improve cellulose nano-fibrous dispersibility, parent
One of aqueous and hydrophobicity or a variety of surfaces characteristic.
It preferably, further include being centrifuged cellulose nano-fibrous dispersion liquid after carrying out nanofiber processing
Separation, then by the cellulose nano-fibrous freezen protective of gained sediment, or by the cellulose nano-fibrous freeze-drying of the sediment
Or drying saves.
Preferably, biomass material includes crop material, branch or timber, bamboo, fiber crops, reed, agricultural product shell and open country
One of plant plant is a variety of, and wherein crop material includes corn stover, straw, sugarcane bar, bagasse and straw
One of or it is a variety of, agricultural product shell includes one of coconut husk, banana crust and beanpod or a variety of.
The present invention combines chemical separation and purification process with physics method for making Nano, effectively improves preparation method
Efficiency prepares the cellulose nano-fibrous of high-purity high length-diameter ratio (length of fiber and the ratio of width are high).In addition, due to
The present invention mixes in chemical separation process using aqueous formic acid or acetic acid aqueous solution or formic acid and acetic acid aqueous solution
This kind of organic acid soln system can further recycle it, to reduce the generation of chemical contamination waste；Together
When, it is avoided in traditional method for bleaching one caused by the use of chlorine using the processing that hydrogenperoxide steam generator bleaches sample
Serial environmental problem.
Detailed description of the invention
Fig. 1 is sweeping for the high-purity high length-diameter ratio wheat straw fiber element nanofiber prepared using the embodiment of the present invention six
Retouch electron microscope image.
Specific embodiment
Technical solution of the present invention is set forth below in conjunction with attached drawing and preferred embodiment.It should be understood that with
Under the embodiment enumerated be merely to illustrate and explain the present invention, without constituting the limitation to technical solution of the present invention.
A method of it is prepared based on biomass material cellulose nano-fibrous, comprising:
Biomass material is dried and micronization processes, the biological material and organic acid solvent for then generating processing
Hybrid Heating reflux separating biomass cellulose, then the biomass cellulose isolated is subjected to nanofiber using physical method
Change processing, obtains the cellulose nano-fibrous of high-purity high length-diameter ratio.Before nanofiberization processing, can will through dry and
The biological material of micronization processes carries out pretreatment of rising brokenly；And/or it can be purified after separating biomass cellulose
Processing.After nanofiberization processing, cellulose nano-fibrous carry out surface modification treatment can be enabled into cellulose
The preparation better effect of nanofiber；And/or it is centrifuged cellulose nano-fibrous, freeze, be lyophilized or drying and processing.
The specific method is as follows:
(1) by biomass material drying and micronization processes；
Such as by crop material (including corn stover, straw, sugarcane bar or bagasse, straw etc.), branch or timber,
Bamboo, fiber crops, reed, agricultural product shell (including coconut husk, banana crust, beanpod etc.) and wild plant plant etc., in nature
It is lower to air-dry or dried under the conditions of 30~65 DEG C；
One of optional following method of the process that biomass material is refined, however it is not limited to listed method: by biomass
Raw material crushed 0.2-5mm sieve into powdered biomass；Or biomass material is rubbed with physical method into suede, and it is raw to obtain elongated fibers
Material.
(2) biological material through dry and micronization processes is subjected to pretreatment of rising brokenly；
Moisten pretreatment of rising including impregnate with physical method steam blasting or chemically 15~20% lye,
It is not limited to this two methods；Consider environmental protection factor, the steam explosion method pretreatment of preferable physics, concrete operations
Are as follows:
Object will be passed through 10~5000g of powdered biomass in step (1) after drying and crushing is sieved or in step (1)
Reason method rub at suede 10~5000g of biological material be packed into reaction vessel in, under 0.5~10.0MPa pressure condition into
Row steam blasting is washed the hydrolyzate generated in the product centrifuge separation removal blasting process after explosion and with distilled water
To neutrality, freeze-drying or supercritical drying processing are finally carried out, the biological material containing biomass cellulose is obtained.
The preprocessing process makes the purity of the cellulose in biological material higher, so that subsequent processing be made to reach more excellent
Effect.In practical applications, the processing can be accepted or rejected as needed.
(3) biomass cellulose in separating biomass material；
Including being separated with organic acid solvent, is perhaps separated with enzyme hydrolysis or is separated etc. with mineral acid hydrolysis, however it is not limited to
Listed method.Since organic acid solvent can recycle, environmental factor and economic benefit are comprehensively considered, it can be preferably with organic
Sour solvent is separated, method particularly includes:
By biological material and aqueous formic acid or arboxylic acid aqueous solution mix reagent pretreated in step (2)
It is mixed with 1: 5~1: 70, wherein formic acid volume content is 5~95%, and acetic acid volume content is 0~95%, and water volume contains
Amount for 5~80% (more excellent volume ratio group is combined into { 20%, 60%, 20% }, { 80%, 0,20% }, { 20%, 70%, 10% },
{ 10%, 80%, 10% } etc., however it is not limited to this)；
The solidliquid mixture is heated to reflux 1~8h under the conditions of 50~107 DEG C, while with the speed of 200~1000rpm
Carry out magnetic-type or mechanical stirring；After reacting stopping, product is cooled to room temperature, with 2000~8000rpm centrifugation 2~
20min is separated, or No. 3 (aperture is 15~40 μm) or No. 4 (aperture is 5~15 μm) sand core funnels is used to be separated by filtration,
And isolate is washed 4~8 times to neutrality with distilled water.
(4) biomass cellulose is purified；
Including purifying (bleaching) processing with hydrogenperoxide steam generator, or with chlorinated solvents chlorite solution or hypochlorite
Solution purification processing, or with inorganic alkali solution purification process etc., however it is not limited to listed method.It, can be excellent in view of environmental factor
Hydrogenperoxide steam generator is selected to carry out purification process to biomass cellulose.The specific method is as follows:
By biomass fiber cellulosic material and 0.5~5% hydrogenperoxide steam generator (pH=9~11) with solid-to-liquid ratio for 1: 5~1:
70 are mixed, and are reacted 1~8 hour under the conditions of 30~80 DEG C, are washed with distilled water 4~8 times to neutrality.In order to improve peroxide
Change the bleaching effect of hydrogen, molybdate, cyanamide, metal complex, biological enzyme etc. can also be added in solution and mentioned as catalyst
Its high purification efficiency.
The purification process process is in order to enable the purity of biomass cellulose further increases, so that subsequent processing be made to reach
To more excellent effect.In practical applications, the processing can be accepted or rejected as needed.
(5) biomass cellulose is subjected to nanofiber processing using physical method；
Physical method said herein, including high-pressure homogeneous microjet is used, or using ultrasound, or recycle using rotary cutting
Grinding, or biomass cellulose sample is subjected to nanosizing processing using technologies such as high-speed homogenizations, however it is not limited to listed method.Its
In, each method process is as follows:
The concentration that biomass cellulose sample is made into 0.01~5% is passed through into high-pressure homogeneous microfluidizer in 50~400MPa
It is handled 1~10 time under pressure, obtains cellulose nano-fibrous dispersion liquid.
The concentration that biomass cellulose sample is made into 0.1~60% is rotated by rotary cutting circular grinding equipment
Circular grinding is cut, or is handled by the even paddle of high speed for the even oarage that flows back at a high speed, cellulose nano-fibrous dispersion liquid is obtained.
(6) cellulose nano-fibrous progress surface is modified；
Using one of following methods or a variety of to cellulose nano-fibrous carry out surface modification treatment: absorption surface is living
Property agent or polyelectrolyte, esterification, etherificate, oxidation, silanization and graft copolymerization, to improve cellulose nano-fibrous dispersion
One of property, hydrophily and hydrophobicity or a variety of surfaces characteristic.The wherein process of oxidation modification specifically:
By the cellulose nano-fibrous sample slurries and 2 by nanofiberization processing, 2,6,6- tetramethyl piperidine -1- oxygen
Free radical (TEMPO)/sodium bromide (NaBr) mixed liquor (mixed proportion 1: 3~1: 10) according to 2: 1~50: 1 volume ratio
It is sufficiently mixed, adjusting and keep the pH of mixture is 9~11, and mixing is mixed using 2% sodium hypochlorite (NaClO) as initiator
Body, and be stirred at room temperature and be modified reaction.To after reaction, surface-modified slurries be filtered and are washed into
Property.
The surface modification treatment is in order to enable biomass cellulose obtains dispersibility, hydrophily or hydrophobicity.In reality
In, the processing can be accepted or rejected as needed.
(7) it separates cellulose nano-fibrous in dispersion liquid.
Cellulose nano-fibrous dispersion liquid is centrifuged, then by gained sediment --- it is cellulose nano-fibrous
Freezen protective, or it is saved after freeze-drying.
Step (2), the main purpose of (4) in the present invention be improve biomass cellulose purity, step (6) be in order to
Cellulose nano-fibrous hydrophily, hydrophobicity and dispersibility are improved, can selectively be accepted or rejected in actual application
Using.
The present invention prepares the high major diameter of high-purity by combining chemical separation and purification process with physics method for making Nano
Ratio it is cellulose nano-fibrous, to improve the purity of preparation, quality and yield.In addition, the present invention is in chemical separation process
Employed in aqueous formic acid or arboxylic acid aqueous solution mix reagent system can further recycle, to reduce
The generation of chemical contamination waste；Hydrogenperoxide steam generator carries out purifying bleaching to sample and avoids in traditional method for bleaching
The use of chlorine and its caused environmental problem.
Embodiment one
Bagasse waste is dried at 45 DEG C, is rubbed into suede；Take the bagasse powder 1000g under 2.0MPa pressure
Steam blasting, centrifugal treating are carried out, and is washed product 5 times with distilled water, is freeze-dried spare；After weighing the freeze-drying
Product 15g (dry weight), with arboxylic acid aqueous solution mix reagent (formic acid/acetic acid/water volume ratio 10/70/20) mix reagent with
Solid-to-liquid ratio 1: 30 is mixed, and 3h is heated to reflux under the conditions of 100 DEG C, while being stirred with the speed of 400rpm；Wait react
Stop, product is cooled to room temperature, filtered with No. 4 (aperture is 5-15 μm) sand core funnels and is washed with distilled water to neutrality；It will
Products therefrom is mixed with 1.5% hydrogen peroxide (pH=10.0) with solid-to-liquid ratio 1: 30, uses distillation after 3h is reacted under the conditions of 55 DEG C
Water washing reaction product is to neutrality；Product sample is made into 0.15% suspension, makes it uniformly through high-pressure homogeneous micro-
Processing 4 times is centrifuged in jet machine under 180MPa pressure；It will centrifuge separation products therefrom freeze-drying；Then it will receive
Riceization product mixes with wooden Portugal oligosaccharide-polyethylene glycol benzene alkene triblock copolymer and carries out adsorption of modification processing, is dispersed
The good high-purity of property, high length-diameter ratio Bagasse-cellulose nanofiber.
Embodiment two
Straw is air-dried under field conditions (factors), crushed 1mm sieve；Take the straw powder sample 2000g in 2.8MPa pressure
Lower progress steam blasting, centrifugal treating, and washed product 5 times with distilled water, it is freeze-dried spare；After weighing the freeze-drying
Product 20g (dry weight), with arboxylic acid aqueous solution mix reagent (formic acid/acetic acid/water volume ratio 5/80/15) mix reagent with
Solid-to-liquid ratio 1: 20 is mixed, and 4h is heated to reflux under the conditions of 90 DEG C, while being stirred with the speed of 350rpm；Stop wait react
Only, product is cooled to room temperature, is then centrifugated with 4500rpm, and be washed with distilled water to neutrality；By products therefrom with
3%NaOH solution is with the mixing of solid-to-liquid ratio 1: 50 and the heating stirring 2h at 80 DEG C；Product sample is made into 0.20% suspension
Liquid makes it uniformly through high-pressure homogeneous microfluidizer, handles 1 time under 200MPa pressure；It will centrifuge separation products therefrom freezing
It is dry；Then nanosizing product is mixed with TEMPO/NaBr (volume ratio 1: 4) according to 10: 1 mixed proportion, adjusts and keeps
The pH value of mixture is 9, and is placed in mixture by initiator of 2%NaClO, is stirred at room temperature and is modified reaction, obtains
Dispersed straw cellulose nanofiber well.
Embodiment three
Wheat stalk is air-dried under field conditions (factors), crushed 1mm sieve；Wheat stalk powder 10g (dry weight) is weighed, with
Arboxylic acid aqueous solution mix reagent (formic acid/acetic acid/water volume ratio 30/50/20) mix reagent is mixed with solid-to-liquid ratio 1: 25, and
It is heated to reflux 3h under the conditions of 107 DEG C, while being stirred with the speed of 400rpm；Stop wait reacting, product is cooled to room
Then temperature is filtered with No. 3 (aperture is 15-40 μm) sand core funnels and is washed with distilled water to neutrality；By products therefrom and 1.8%
- 0.18% cyanamide solution (pH=10.0) of hydrogen peroxide uses distillation after reacting 4h under the conditions of 50 DEG C with the mixing of solid-to-liquid ratio 1: 30
Water washing is to neutrality；Product sample is made into 0.10% suspension, makes it uniformly through high-pressure homogeneous microfluidizer,
It is handled 5 times under 150MPa pressure, obtains wheat straw fiber element nanofiber dispersion liquid；The wheat being centrifugated in the dispersion liquid
Stalk cellulose nanofiber, then freeze-drying saves.
Example IV
Corn stover is dried at 65 DEG C, crushed 1mm sieve；Take maize straw powder 50g under 2.5MPa pressure
Steam blasting, centrifugal treating are carried out, and is washed product to neutrality with distilled water, is freeze-dried spare；Weigh the freeze-drying
Product 10g afterwards is reacted 90 minutes at 40 DEG C using zytase；Stop wait reacting, reaction life is centrifugated with 2000rpm
At object and it is washed with distilled water to neutrality；By products therefrom and -0.15% sodium molybdate solution of 2.0% hydrogen peroxide (pH=10.0)
With the mixing of solid-to-liquid ratio 1: 30, reaction product is washed to neutrality with distilled water after reacting 3h under the conditions of 55 DEG C；By product sample
Product are made into 0.25% suspension, make it uniformly through high-pressure homogeneous microfluidizer, handle 6 times, obtain under 140MPa pressure
Corn stalk fiber element nanofiber dispersion liquid；The corn stalk fiber element nanofiber being centrifugated in the dispersion liquid, then
Freeze-drying saves.
Embodiment five
Cotton stem is air-dried under field conditions (factors), crushed 1mm sieve；The cotton stem powder sample 800g is taken to press in 2.2MPa
Steam blasting, centrifugal treating are carried out under power, and is washed product to neutrality with distilled water, are freeze-dried spare；Weigh the freezing
Product 5g (dry weight) after drying is mixed with arboxylic acid aqueous solution mix reagent (formic acid/acetic acid/water volume ratio 60/30/10)
Reagent is mixed with solid-to-liquid ratio 1: 30,1h is heated to reflux under the conditions of 100 DEG C, while being stirred with the speed of 400rpm；
Stop wait reacting, reaction product is cooled to room temperature, then filtered with No. 4 (aperture is 5-15 μm) sand core funnels and uses distilled water
It washs to neutrality；Products therefrom and -0.05% cyanamide solution (pH=10.0) of 0.5% hydrogen peroxide is mixed with solid-to-liquid ratio 1: 70
It closes, is washed with distilled water to neutrality after reacting 4h under the conditions of 50 DEG C；Product sample is made into 0.12% suspension, makes it
It is handled 10 times under 200MPa pressure uniformly through high-pressure homogeneous microfluidizer；It is centrifugated the product of nanosizing, and is freezed dry
It is dry；Product after freeze-drying acetate or sulfuric ester or maleate are subjected to graft modification, obtained dispersed fine
High-purity cotton stem it is cellulose nano-fibrous.
Embodiment six
Wheat stalk is air-dried under field conditions (factors), crushed 1mm sieve；Wheat stalk powder sample 500g is taken to exist
Steam blasting, separating treatment are carried out under 2.5MPa pressure, and is washed product to neutrality with distilled water, are freeze-dried spare；Claim
Product 10g (dry weight) after taking the freeze-drying, with arboxylic acid aqueous solution mix reagent (formic acid/acetic acid/water volume ratio 30/
50/20) mix reagent is heated to reflux 3h with the mixing of solid-to-liquid ratio 1: 25 under the conditions of 107 DEG C, while with the progress of the speed of 400rpm
Stirring；Stop wait reacting, reaction product is cooled to room temperature, is then filtered and be used in combination with No. 3 (aperture is 15-40 μm) sand core funnels
Water washing is distilled to neutrality；By products therefrom and -0.18% cyanamide solution (pH=10.0) of 1.8% hydrogen peroxide with solid-to-liquid ratio 1:
30 mixing, are washed with distilled water to neutrality after reacting 4h under the conditions of 50 DEG C；Product sample is made into 0.10% suspension,
It handles it 5 times under 150MPa pressure uniformly through high-pressure homogeneous microfluidizer, obtains wheat straw fiber element nanofiber
Dispersion liquid；It is centrifugated the dispersion liquid and obtains wheat straw fiber element nanofiber, then freeze-drying saves.
Embodiment seven
Corn stover or straw or sugarcane bar or bagasse or straw or reed are air-dried under field conditions (factors), and crushed
0.2mm sieve；Powder sample 4000g is taken to carry out steam blasting, centrifugal treating under 2.8MPa pressure, and with distilled water by product
Washing 5 times is freeze-dried spare；Product 100g (dry weight) after weighing the freeze-drying, with aqueous formic acid (formic acid/water body
Product is mixed than 95/5) mix reagent with solid-to-liquid ratio 1: 60, is heated to reflux 8h, while under the conditions of 50 DEG C with the speed of 350rpm
Degree is stirred；Stop wait reacting, reaction product is cooled to room temperature, then with No. 3 (aperture is 15-40 μm) sand core funnel mistakes
It filters and is washed with distilled water to neutrality；Products therefrom is mixed with -0.4% ammonium molybdate of 4% hydrogen peroxide according to 1: 10,
Stirring bleaching was washed with distilled water to neutrality after 8 hours under the conditions of 35 DEG C；Product after purification is made into 60% suspension, is made
It is handled by rotary cutting circular grinding machine, obtains corn stover or straw or sugarcane bar or bagasse or straw or reed
Cellulose nano-fibrous dispersion liquid；It is centrifugated the dispersion liquid and obtains corresponding cellulose nano-fibrous, then freeze-drying is protected
It deposits.
Embodiment eight
Branch or timber or bamboo are air-dried under field conditions (factors), crushed 5mm sieve；Powder sample 10g (dry weight) is weighed,
It is mixed with arboxylic acid aqueous solution mix reagent (formic acid/acetic acid/water volume ratio 5/90/5) mix reagent with solid-to-liquid ratio 1: 5,
It is heated to reflux 6h under the conditions of 70 DEG C, while being stirred with the speed of 400rpm；Stop wait reacting, reaction product is cooled to room
Then temperature is filtered with No. 3 (aperture is 15-40 μm) sand core funnels and is washed with distilled water neutrality；By products therefrom and 5% peroxide
Change hydrogen solution (pH=11.0) with the mixing of solid-to-liquid ratio 1: 10, is washed with distilled water to neutrality after reacting 1h under the conditions of 80 DEG C；It will
Product sample is made into 15% suspension, and high speed reflux homogenized is carried out to it, obtains the fiber of branch or timber or bamboo
Plain nanofiber dispersion liquid；It is centrifugated the dispersion liquid and obtains corresponding cellulose nano-fibrous, then freeze-drying preservation.
Embodiment nine
Coconut husk or banana crust or beanpod are dried at 30 DEG C, crushed 2mm sieve；Take powder 1000g with 17.5%
NaOH solution impregnate 2h profit rise, centrifugal treating, and be washed with distilled water to neutrality, be freeze-dried spare；By the freeze-drying
Product and arboxylic acid aqueous solution mix reagent (formic acid/acetic acid/water volume ratio 40/40/20) mix reagent with solid-to-liquid ratio 1:
50 are mixed, and 5h are heated to reflux under the conditions of 80 DEG C, while being stirred with the speed of 450rpm；Stop wait reacting, it will be anti-
It answers product to be cooled to room temperature, then filtered with No. 3 (aperture is 15-40 μm) sand core funnels and is washed with distilled water to neutrality；It will
Product sample is made into 0.25% suspension, it is made to handle 6 under 140MPa pressure uniformly through high-pressure homogeneous microfluidizer
It is secondary；It is centrifugated the product of nanosizing, is then freeze-dried；Product after freeze-drying is carried out grafting with trimethyl silane to change
Property obtains the coconut husk or banana crust or hull fiber element nanofiber of favorable dispersibility.
Embodiment ten
Weeds plant is air-dried under field conditions (factors), is rubbed into suede；The rubbing is weighed at the product 5g (dry weight) of suede, with first
Sour acetic acid aqueous solution mix reagent (formic acid/acetic acid/water volume ratio 60/30/10) mix reagent is mixed with solid-to-liquid ratio 1: 30,
It is heated to reflux 4h under the conditions of 100 DEG C, while being stirred with the speed of 400rpm；Stop wait reacting, reaction product is cooling
To room temperature, is then filtered with No. 4 (aperture is 5-15 μm) sand core funnels and be washed with distilled water neutrality；By products therefrom and 5%
Sodium chlorite (pH=4.0) solution is washed with distilled water to neutrality after reacting 3h under the conditions of 50 DEG C with the mixing of solid-to-liquid ratio 1: 30；
Product sample is made into 5% suspension, handles it in processor for ultrasonic wave 0.5 hour, weeds cellulose is obtained and receives
Rice fiber dispersion；It is centrifugated the dispersion liquid and obtains corresponding cellulose nano-fibrous, then freeze-drying preservation.
Embodiment 11
Barley straw is air-dried under field conditions (factors), crushed 1mm sieve；Take powder 5000g under 2.5MPa pressure into
Row steam blasting, separating treatment, and it is washed with distilled water to neutrality, it is freeze-dried spare；Weigh the product 50g of the freeze-drying
(dry weight), with 1M H2SO4Solution heats 3h with the mixing of solid-to-liquid ratio 1: 25 under the conditions of 80 DEG C, at the same with the speed of 400rpm into
Row stirring；Stop wait reacting, reaction product is cooled to room temperature, is centrifugated with 8000rpm and is washed with distilled water neutrality；It will
Products therefrom is mixed with 1% hydrogenperoxide steam generator (pH=10.0) with solid-to-liquid ratio 1: 50, uses steaming after 4h is reacted under the conditions of 60 DEG C
Distilled water is washed to neutrality；Product sample is made into 30% suspension, is handled using rotary cutting circular grinding equipment；Centrifugation
The product of nanosizing is separated, and is freeze-dried；Products therefrom and TEMPO/NaBr (1: 8) are sufficiently mixed according to 40: 1, are adjusted simultaneously
Keeping pH is 11, is placed in, and be stirred at room temperature and be modified reaction by initiator of 2%NaClO, obtains favorable dispersibility
Barley straw is cellulose nano-fibrous.
Table 1 indicate be in above-described embodiment three, six after variety of processes in product cellulose purity variation.
Table 1
Claims (7)
1. a kind of prepare cellulose nano-fibrous method based on biomass material, comprising: biomass material is dried and
Micronization processes, and steam blasting pretreatment, the biology that then will be obtained are carried out to the biological material after drying and micronization processes
Material and organic acid solvent Hybrid Heating reflux separating biomass cellulose, then with hydrogenperoxide steam generator to the biomass
Biomass cellulose in material carries out purification process；The biomass cellulose of purified processing is carried out using physical method again
Nanofiberization processing, obtains the cellulose nano-fibrous of high-purity high length-diameter ratio；The above-mentioned biological material that will be obtained with have
Machine sour solvent Hybrid Heating reflux separating biomass cellulose, specifically: by the biological material and aqueous formic acid or first
One of sour acetic acid water mixed solution reagent is mixed with 1:5~1:70, and wherein the volume content of formic acid is 5~95%,
The volume content of acetic acid is 0~95%, and the volume content of water is 5~80%；It is above-mentioned with hydrogenperoxide steam generator to the biomass
Biomass cellulose in material carries out purification process, specifically: being 9 by biomass fiber cellulosic material and 0.5~5% and pH value
~11 hydrogenperoxide steam generator is mixed with solid-to-liquid ratio for 1:5~1:70, and is reacted 1~8 hour under the conditions of 30~80 DEG C,
4~8 times are washed with distilled water to neutrality；It is above-mentioned that biomass material is dried and micronization processes, it specifically includes: by the life
Raw material of substance is air-dried in its natural state or is dried under the conditions of 30~65 DEG C, then, by the air-dried or described drying
Biomass material pulverizes and sieves to obtain powdered biological material, or the biomass original that will be air-dried or be dried with physical method
Material rubbing is at velvet-like biological material；The above-mentioned biological material to after drying and micronization processes carries out steam blasting and locates in advance
Reason, detailed process are as follows: by pulverize and sieve described in process generation powdered 10~5000g of biological material or pass through described in rub
Velvet-like 10~the 5000g of biological material for being twisted into generation is packed into reaction vessel, is carried out under 0.5~10.0MPa pressure condition
Steam blasting, the hydrolyzate that then will be generated in the centrifuge separation removal blasting process of the product after explosion, and will be divided with distilled water
It leaves away except the product after hydrolyzate is washed to neutrality, then washing to neutral product is carried out at freeze-drying or supercritical drying
Reason, obtains the biological material containing biomass cellulose.
2. according to the method for claim 1, which is characterized in that after carrying out the nanofiberization processing, further include
By cellulose nano-fibrous carry out surface modification treatment, which includes one of following methods or a variety of: being adopted
With absorption surface activating agent, absorption polyelectrolyte, esterification, etherificate, oxidation, silanization and graft copolymerization.
3. according to the method for claim 1, which is characterized in that it is described that nanofiber processing is carried out using physical method,
Including one of following method: using high-pressure homogeneous microjet method, or use ultrasonic method, or use rotary cutting circular grinding
Method, or use high-speed homogenization method.
4. according to the method for claim 3, which is characterized in that specifically included: will be given birth to using high-pressure homogeneous microjet method
The concentration that material fibrils element sample is made into 0.01~5% handles 1 under 50~400MPa pressure by high-pressure homogeneous microfluidizer
~10 times, obtain cellulose nano-fibrous dispersion liquid.
5. according to the method for claim 4, which is characterized in that after carrying out the nanofiberization processing, further include
Cellulose nano-fibrous dispersion liquid is centrifuged, then by the cellulose nano-fibrous freezen protective of gained sediment, or
Person saves the cellulose nano-fibrous freeze-drying of the sediment or drying.
6. according to method described in any one of claim 1 to 5, which is characterized in that the biomass material include crop material,
One of timber, bamboo, fiber crops, agricultural product shell and wild plant plant are a variety of.
7. according to the method for claim 6, which is characterized in that the crop material includes corn stover, straw, sugarcane bar
One of waste and straw are a variety of, the agricultural product shell include one of coconut husk, banana crust and beanpod or
It is a variety of；The wild plant plant includes reed.
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