CN109868667A - A kind of preparation method of the fibril of nano-cellulose containing lignin - Google Patents
A kind of preparation method of the fibril of nano-cellulose containing lignin Download PDFInfo
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- CN109868667A CN109868667A CN201711263843.0A CN201711263843A CN109868667A CN 109868667 A CN109868667 A CN 109868667A CN 201711263843 A CN201711263843 A CN 201711263843A CN 109868667 A CN109868667 A CN 109868667A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of preparation method of fibril of nano-cellulose containing lignin, this method uses Wooden Biomass raw material, economic and environment-friendly, can be mass-produced.It is characterized by comprising the following steps: 1) raw material crushes；2) it is extracted with aqueous slkali；3) wood powder after alkali density directly uses, or takes out partial lignin；4) will treated wood powder by cellulase degradation processing；5) wood powder handled more than is made into water slurry, is ground with grinder, and the controllable nano-cellulose fibril aqueous solution of content of lignin is obtained.The present invention uses mechanical milling method, and preparation has green non-pollution, energy-saving and environment-friendly lignin-nano-cellulose solution, and this method meets the environmentally protective requirement of modern society.
Description
Technical field
The present invention relates to a kind of preparation methods of fibril of nano-cellulose containing lignin, and this method is environmentally protective, operation is simple
Easily, the nano-cellulose fibril of acquisition belongs to natural polymer subdomains, also belongs to Forestry Engineering, Packaging Engineering, new material neck
Domain.
Background technique
Cellulose and lignin are renewable organic resources abundant in nature, are widely present in plant material, are
The main component of timber belongs to renewable natural macromolecular material inexhaustible in nature.Lignocellulosic
With its excellent characteristic (high-crystallinity, degradable, high-intensitive, high-hydrophilic and biocompatibility etc.), it is widely used in
The fields such as weaving, paper pulp, wood hydrolysis, biological material, biomass energy, biological medicine, building.With nanoscale science and technology
Fast development, the preparation of nano-cellulose fibril and application also attract attention, and this resource is cheap, from a wealth of sources, green can
The new material that lasting new resources are formed on nanoscale has excellent physicochemical property, for example, nano-cellulose fibril table
The small-size effect revealed, quantum effect, skin effect etc. are being catalyzed, and absorption, electromagnetic arts are with a wide range of applications, make
Nano-cellulose fibril becomes a hot research field of current forest-science development.
Currently, the preparation of nano-cellulose fibril mainly includes Mechanical Method, chemical method and three kinds of bioanalysis.Mechanical Method is main
It is to disperse fiber using mechanicals efforts, nanoscale, including polishing, high pressure homogenization method, microjet and freezing powder is presented
It is broken；Chemical rule is the decomposition of cellulose to be realized using acid, alkali and Strong oxdiative reagent, such as acid-hydrolysis method, TEMPO are aoxidized
Method；Biological rule realizes the hydrolysis of cellulose using cellulase, to prepare the cellulose fibril of nanoscale.However, base
In the preparation for the nanofibrils that plant fiber is raw material, lignin is essentially all to be discharged as waste.In nature, wooden
The content of quality is only second to cellulose, removes lignin not only energy consumption with higher, while needing using certain chemistry examination
Agent will cause certain environmental hazard.Although Mechanical Method and the nano-cellulose fibril of bioanalysis preparation do not add any chemistry
Reagent, but the delignification link of early period certainly will will affect the preparation cost of entire nano-cellulose fibril.Therefore, preparation is containing wood
Quality nano-cellulose fibril meets the environmentally protective requirement of modern society.In addition, the nano-cellulose fibril energy containing lignin
Enough slow down the degradation rate of the material, and since lignin itself has uvioresistant function, it can be made to be applied to special anti-purple
The preparation of outer material, this provides new thinking for the value added applications of nano-cellulose fibril.
Summary of the invention
It is an object of the invention to propose a kind of preparation method of fibril of nano-cellulose containing lignin, its object is to subtract
The use of chemical reagent in few nano-cellulose fibril preparation process, reduces energy consumption and production costs, while realizing Nanowire
Tie up the uvioresistant of plain filament material, the functions such as anti-degradation.The present invention is realized using Mechanical Method using wood powder as raw material and contains lignin
The green industrialized production of nano-cellulose fibril, this method is at low cost, and high-efficient, there are no pollution to the environment, and prepared contains
Lignin nano-cellulose fibril can be used for special Electronic Paper, UV resistance film, solar battery etc. with high value added product
Or industry.
The purpose of the present invention is what is be achieved through the following technical solutions:
(1) taking a certain amount of timber is raw material, is crushed using pulverizer, and 60 meshes are crossed.
(2) a certain amount of wood powder is taken, is filtered after 1 ~ 3h of stir process at 70 ~ 90 DEG C with 0.5 ~ 2%NaOH solution, uses water
It rinses to neutrality.
(3) at room temperature, with the distilled water immersion of 50 ~ 100 times of wood powder quality, soaking time is filtered wood powder
It after 10 ~ 24 hours, directly uses, content of lignin is timber maximum level containing lignin at this time；Or will treated wood powder,
The distillation of the sodium chlorite of 0.3 ~ 0.4 times of wood powder quality, the glacial acetic acid of 0.1 ~ 0.3 times of wood powder quality and 25 ~ 35 times of wood powder quality
Water is configured to aqueous solution, reacts 1h at 75 DEG C, repeats and filters after same amount of sodium chlorite and glacial acetic acid 1 ~ 5 time is added,
With distilled water flushing 3 ~ 5 times, partial lignin, control wood are removed by amount and reaction time that sodium chlorite and glacial acetic acid is added
The content of lignin in powder.
(4) treated more than, and raw material directly uses；Or the cellulase of 0.005 ~ 0.06 times of wood powder quality is added, and add
Enter certain mass, the buffer solution that pH is 4.8 ~ 5.5 is placed in 2 ~ 20h of isothermal reaction in≤50 DEG C of shaking table, shaking table concussion frequency
Rate is 150 ~ 180 revs/min, after reaction filters enzymatic hydrolysis wood powder and washs to neutrality, adds a certain amount of distilled water and set
Isothermal vibration reacts 0.5 ~ 1h in 80 ~ 100 DEG C of shaking table, and shaking table oscillation frequency is 150 ~ 180 revs/min, stops enzyme reaction, mistake
Wood powder is filtered, for use.
(5) wood powder, alkali density-delignification wood powder, alkali density-enzymatic hydrolysis wood powder or the alkali density-after alkali density are removed into wood
One of quality-enzymatic hydrolysis wood powder, is formulated directly into the aqueous suspension of solid content≤2%, is then ground, and grinding turns
Speed is 1500rpm, >=0 rough lapping, milling gap -50 ~ -200 μm is first carried out, then carry out >=1 fine lapping, between grinding
Gap -200 ~ -300 μm.
(6) it obtains the fibril solution of nano-cellulose containing lignin and is placed in 4 DEG C of refrigerator storages, prevent cellulose solution overheat group
It is poly-.
It in above-mentioned technical proposal, can be used directly with the wood powder after alkaline solution treatment, be made into the aqueous solution of suitable solid content
Directly ground；Wood powder can also be subjected to partial lignin removal, according to the amount and reaction that sodium chlorite and glacial acetic acid is added
Time is different (referring to GB/T 2677.10), obtains the wood powder of different content of lignin, retains content of lignin in wood powder, can lead to
Cross the measurement of national standard GB/T 2677.8；Enzymatic hydrolysis pretreatment can shorten milling time, by be added cellulase dosage and reaction when
Between, reduce rough lapping number.
The present invention has the advantage that the nano-cellulose fibril of 1) this method preparation is sufficiently sharp compared with prior art
With wood raw material, wherein content of lignin is controllably between 0.01% ~ 40%, suitable for the fiber containing different lignin quality scores
The exploitation and preparation of plain nano material.2) this method is easy to operate, and quickly, it is at low cost that low energy consumption, can carry out industrializing extensive
Production, high-efficient, no pollution to the environment are a kind of environmentally protective preparation methods.3) nanometer containing lignin prepared by the present invention
Cellulose fibril diameter is distributed between 5 ~ 30nm, and for length between 0.5 ~ 5 μm, draw ratio is suitable, utilizes scanning electron microscopic observation
In fibril reticular structure.
Detailed description of the invention
Fig. 1 is the SEM picture of the fibril of nano-cellulose containing lignin
Specific embodiment
Advantages of the present invention and other details, but the specific material quoted in embodiment are further illustrated in the examples below
Material and dosage and other conditions should not be regarded as having carried out inappropriate limitation to the present invention.
Embodiment 1
(1) taking 20g poplar is raw material, is crushed with pulverizer, and 60 meshes are crossed.
(2) 10g wood powder is taken, is filtered, is rinsed with water into after stir process 1.5h at 80 DEG C with 0.5% NaOH solution
Property.
(3) filtered wood powder at room temperature, is directly made after impregnating 10h with 1000mL distilled water immersion wood powder
With.
(4) wood powder is formulated directly into the aqueous suspension that solid content is 0.5%, be then ground, grinding revolving speed is
1500rpm, first 5 rough lappings of progress, -100 μm of milling gap, then 25 fine lappings are carried out, -200 μm of milling gap.
(5) it obtains the fibril solution of nano-cellulose containing lignin and is placed in 4 DEG C of refrigerator storages, prevent cellulose solution overheat group
It is poly-.
Embodiment 2
(1) taking 25g Eucalyptus is raw material, is crushed using pulverizer, and 60 meshes are crossed.
(2) 15g wood powder is taken, is filtered, is rinsed with water to neutrality after stir process 1h at 90 DEG C with 1% NaOH solution.
(3) distilled water of the filtered wood powder of 10g, the sodium chlorite of 3.5g, the glacial acetic acid of 2.5g and 300g is taken to be placed in
In 500mL conical flask, filtered after reacting 1h at 75 DEG C, with distilled water flushing 5 times.
(4) treated, and wood powder is formulated directly into the aqueous suspension that solid content is 1%, is then ground, and grinding turns
Speed is 1500rpm, first 10 rough lappings of progress, -150 μm of milling gap, then 5 fine lappings are carried out, -250 μm of milling gap.
(5) it obtains the fibril solution of nano-cellulose containing lignin and is placed in 4 DEG C of refrigerator storages, prevent cellulose solution overheat group
It is poly-.
Embodiment 3
(1) China fir for taking 40g is raw material, is crushed using pulverizer, and 60 meshes are crossed.
(2) 20g wood powder is taken, is filtered, is rinsed with water to neutrality after stir process 3h at 70 DEG C with 1.5% NaOH solution.
(3) filtered wood powder 15g is taken, 0.2g cellulase is added, and the buffer solution that 300mL pH is 4.8 is added
In the conical flask of 500mL, it is placed in isothermal reaction 10h in 50 DEG C of shaking tables, shaking table oscillation frequency is 180 revs/min, and reaction terminates
Enzymatic hydrolysis wood powder is filtered afterwards and is washed to neutrality, the distilled water for adding 100mL is placed in isothermal vibration in 80 DEG C of shaking tables and reacts
30min, shaking table oscillation frequency are 180 revs/min, stop enzyme reaction, filter wood powder.
(4) wood powder will be digested and is directly configured to the aqueous suspension that solid content is 1.5%, be then ground, grinding turns
Speed is 1500rpm, first 2 rough lappings of progress, -50 μm of milling gap, then 3 fine lappings are carried out, -300 μm of milling gap.
(5) it obtains the fibril solution of nano-cellulose containing lignin and is placed in 4 DEG C of refrigerator storages, prevent cellulose solution overheat group
It is poly-.
Embodiment 4
(1) taking 30g pine is raw material, is crushed using pulverizer, and 60 meshes are crossed.
(2) 20g wood powder is taken, is filtered, is rinsed with water to neutrality after stir process 2h at 90 DEG C with 2% NaOH solution.
(3) water of the filtered wood powder of 15g, the sodium chlorite of 0.45g, the glacial acetic acid of 1.5g and 450g is taken to be configured to water-soluble
Liquid, after reacting 1h at 75 DEG C, the glacial acetic acid of the sodium chlorite, 1.5g that continuously add 0.45g filters after reacting 1h again, with distillation
Water rinses 4 times.
(4) treated more than, and 0.6g cellulase is added in wood powder, and the buffer solution that 300mL pH is 5.0 is added, and puts
It is placed in isothermal reaction 20h in 50 DEG C of shaking tables, shaking table oscillation frequency is 170 revs/min, and enzymatic hydrolysis wood powder is filtered and washed after reaction
It washs to neutrality, the distilled water for adding 300mL is placed in isothermal vibration in 80 DEG C of shaking tables and reacts 30min, and shaking table oscillation frequency is 170
Rev/min, stop enzyme reaction, filters wood powder.
(5) by treated, wood powder is formulated directly into the aqueous suspension that solid content is 1.5%, is then ground, grinds
Mill revolving speed is 1500rpm, without rough lapping, directly 10 fine lappings of progress, and -200 μm of milling gap.
(6) it obtains the fibril solution of nano-cellulose containing lignin and is placed in 4 DEG C of refrigerator storages, prevent cellulose solution overheat group
It is poly-.
Embodiment 5
(1) taking 20g poplar is raw material, is crushed using pulverizer, and 60 meshes are crossed.
(2) 10g wood powder is taken, is filtered, is rinsed with water to neutrality after stir process 1h at 90 DEG C with 1%NaOH solution.
(3) water of the filtered wood powder of 8g, the sodium chlorite of 2.4g, the glacial acetic acid of 0.8g and 240g is taken to be configured to water-soluble
Liquid, after reacting 1h at 75 DEG C, the glacial acetic acid of the sodium chlorite, 0.8g that add 2.4g reacts 1h again, repeats the operation one
Filtering after secondary, with distilled water flushing 4 times.
(4) treated more than, and 0.1g cellulase is added in wood powder, and the buffer solution that 160mL pH is 5.5 is added, and puts
It is placed in isothermal reaction 20h in 50 DEG C of shaking tables, shaking table oscillation frequency is 160 revs/min, and enzymatic hydrolysis wood powder is filtered and washed after reaction
It washs to neutrality, the distilled water for adding 200mL is placed in isothermal vibration in 80 DEG C of shaking tables and reacts 30min, and shaking table oscillation frequency is 160
Rev/min, stop enzyme reaction, filters wood powder.
(5) by treated, wood powder is formulated directly into the aqueous suspension that solid content is 1%, is then ground, grinds
Revolving speed is 1500rpm, first 1 rough lapping of progress, -100 μm of milling gap, then 10 fine lappings are carried out, -300 μm of milling gap.
(6) it obtains the fibril solution of nano-cellulose containing lignin and is placed in 4 DEG C of refrigerator storages, prevent cellulose solution overheat group
It is poly-.
Claims (8)
1. a kind of preparation method of the fibril of nano-cellulose containing lignin, it is characterised in that: the following steps are included:
Raw material: using timber as raw material；
Alkali density processing: wood powder is taken, with being filtered after NaOH solution immersion treatment, is rinsed with water to neutrality；
Delignification processing: will treated that wood powder is added to sodium chlorite, glacial acetic acid and distilled water is configured in aqueous solution instead
It answers, sodium chlorite and glacial acetic acid control removal content of lignin is added by repeating, filters, is rushed with distilled water after the reaction was completed
It washes；
Enzyme pretreatment: by wood powder, cellulase and buffer solution isothermal reaction, after enzymatic hydrolysis wood powder is filtered and is washed into
Property, it adds distilled water and is placed in shaking table high temperature concussion reaction, stop enzyme reaction, filter wood powder；
Milled processed: by treated, wood powder is formulated directly into aqueous suspension, using grinder milled processed, obtains containing lignin
Nano-cellulose fibril aqueous solution.
2. a kind of preparation method of the fibril of nano-cellulose containing lignin as described in claim 1, it is characterised in that: step
(1) raw material is poplar, Eucalyptus, pine, China fir, and wood powder is ground into use process, crosses 60 meshes.
3. a kind of preparation method of the fibril of nano-cellulose containing lignin as described in claim 1, it is characterised in that: step
(2) alkali density described in handles the NaOH solution of 0.5 ~ 2% mass fraction, 1 ~ 3h of stir process at 70 ~ 90 DEG C.
4. a kind of preparation method of the fibril of nano-cellulose containing lignin as described in claim 1, it is characterised in that: step
(3) sodium chlorite used when the processing of delignification described in is 0.3 ~ 0.4 times of wood powder quality, and glacial acetic acid is wood powder quality
0.1 ~ 0.3, distilled water is 25 ~ 35 times of wood powder quality, and reaction temperature is 60 ~ 80 DEG C, and the single reaction time is 1h, repeats and adds
Enter same amount of sodium chlorite and glacial acetic acid 1 ~ 5 time, with distilled water flushing 3 ~ 5 times.
5. a kind of preparation method of the fibril of nano-cellulose containing lignin as described in claim 1, it is characterised in that: step
(4) cellulase used when enzyme pretreatment described in is 0.005 ~ 0.06 times of wood powder quality, buffer solution pH is 4.8 ~
5.5, shaking table temperature≤50 DEG C, 2 ~ 20h of isothermal reaction, shaking table oscillation frequency is 150 ~ 180 revs/min, after reaction enzymatic hydrolysis wood
Amidin shakes in shaking table high temperature, and 80 ~ 100 DEG C of temperature, the reaction time is 0.5 ~ 1h, and shaking table oscillation frequency is 150 ~ 180
Rev/min.
6. a kind of preparation method of the fibril of nano-cellulose containing lignin as described in claim 1, it is characterised in that: step
(5) raw material that milled processed process uses in can be alkali density treated wood powder, alkali density-delignification treated wood
Any one in the wood powder after wood powder or alkali density-delignification-enzymatic hydrolysis three step process after powder, alkali density-enzymolysis processing.
7. a kind of preparation method of the fibril of nano-cellulose containing lignin as described in claim 1, it is characterised in that: step
(5) the milled processed process described in, aqueous suspension solid content are not higher than 2%.
8. a kind of preparation method of the fibril of nano-cellulose containing lignin as described in claim 1, it is characterised in that: step
(5) the milled processed process described in, rough lapping number >=0 time, milling gap -50 ~ -200 μm, fine lapping number >=1 time are ground
Grind gap -200 ~ -300 μm.
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| CN110438833A (en) * | 2019-06-20 | 2019-11-12 | 浙江金加浩绿色纳米材料股份有限公司 | A kind of preparation method of nanofiber degradable fruit tray |
| CN112160179A (en) * | 2020-09-04 | 2021-01-01 | 西南大学 | Preparation method of pineapple peel residue lignocellulose |
| CN112252068A (en) * | 2020-09-01 | 2021-01-22 | 华南理工大学 | Lignocellulose nanofibrils as well as preparation method and application thereof |
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