CN107936125A - A kind of preparation method of micro-nano cellulose - Google Patents
A kind of preparation method of micro-nano cellulose Download PDFInfo
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- CN107936125A CN107936125A CN201711306153.9A CN201711306153A CN107936125A CN 107936125 A CN107936125 A CN 107936125A CN 201711306153 A CN201711306153 A CN 201711306153A CN 107936125 A CN107936125 A CN 107936125A
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
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Abstract
A kind of preparation method of micro-nano cellulose, is related to macromolecule material preparation area.After plant fiber is crushed impurity and dissolved lignin are washed away with NaOH pretreatments；Pretreated fiber dust is filtered out, it is dry after washing to neutrality；Pretreated fiber dust is used into mineral acid hydrolysis again, then separates and collects spent acid and micro-nano cellulose dope, micro-nano cellulose dope is washed to neutrality, is finally freeze-dried micro-nano cellulose dope, up to micro-nano cellulose.Micro-nano cellulose odorlessness, tasteless, not soluble in water and organic solvent prepared by the present invention, particle diameter are corynebacterium, and micro-nano cellulose good dispersion, stability height, yield reach as high as 71.4% within 50 μm.And caused spent acid can reuse after simple process in preparation process, reduce the pollution to environment；Whole preparation process is easy to operate, and cost is low, and energy consumption is low.
Description
Technical field
The present invention relates to a kind of method that micro-nano cellulose is prepared with plant fiber, belongs to high molecular material and prepares neck
Domain.
Background technology
Cellulose is a kind of very abundant renewable resource, while is also a kind of natural macromolecular material.Since it can
The advantages that regenerating, is pollution-free, receives more and more attention in recent years.Plant cellulose can pass through Mechanical Method, chemical method or life
It is prepared by thing method etc..Micro-nano cellulose has many excellent performances, such as larger specific surface area, high-hydrophilic, high intensity,
High-modulus, high-crystallinity and high polymerization degree etc., in view of these excellent performances that micro-nano cellulose has, its chemical industry, food,
The fields such as medicine, material have good potential use and utility value.
The preparation method of the micro-nano cellulose of document report mainly has at present：
CN201410403739.7 discloses a kind of preparation method of micro-nano cellulose, its use the method for pure physics come
Prepare micro-nano cellulose, native cellulose is first destroyed its immanent structure through high-energy electron beam irradiation, then it is thick with machinery dry method
These cellulosic materials Jing Guo radiation treatment are crushed, then become more meticulous crushing to it with levigation method again to obtain micro nanometer fiber
Element.This method is environmentally safe, but prepared by its pure physical method, and technics comparing is complicated, higher to equipment requirement, consume energy compared with
Greatly, it is not suitable for mass producing.
CN201610041262.1 discloses a kind of high-pressure homogeneous nano-cellulose fibril for preparing of formic acid pretreatment joint
Cellulosic material is first added to heating stirring in formic acid solution and hydrolyzes the cellulose that is pre-processed by method, this method, then will
The cellulose of pretreatment is made into cellulose suspension, then carries out homogenization with high pressure homogenizer again, finally obtains gelatinous
Nano-cellulose fibril product.High pressure homogenizer has become at present prepares the common mechanical means of micro-nano cellulose, but
Blocking is be easy to cause when preparing micro-nano cellulose with this kind of method, and obtained product size is uneven, generally requires repeatedly
Repeat high-pressure homogeneous.
CN201310081960.0 discloses a kind of method for preparing nano-cellulose, and this method is in the pre- Xie Chu of plant fiber
TEMPO (2,2,6,6- tetramethyl -1- piperidines-N- oxygen radicals and its derivative) is added during reason and carries out catalysis oxidation, to oxidation
Fiber afterwards carries out defibrating processing until obtaining freedom reaches 50ml and following oxidized fibre, then to oxidized fibre progress
Nanosizing processing, finally obtains nano-cellulose solution.Nano-cellulose is prepared with this method, due to TEMPO expensive catalysts
And it is difficult to carry out recycling, institute's higher industrialized production difficult to realize of cost in this way.
CN201110002108.0 discloses a kind of method for the bio-mechanical sub-wire for manufacturing nano-cellulose, and this method will
Paper pulp is immersed in sugar aqueous solution, and the wheat bran, peptone, yeast for adding certain weight ratio ferment, to fermentation slurry after fermentation
Repeat to grind, prepare nano-cellulose colloidal solution, then filtering, vacuum freeze drying obtain nano-cellulose；It is but this
Method prepares that nano-cellulose reaction efficiency is low, the reaction time is longer.
CN201610753659.3 discloses a kind of preparation method of micro-nano cellulose, this method by cellulosic material with
Buffer solution, biology enzyme mix, and filtering high temperature inactivates after enzymolysis, then refines defibrination again, finally carry out high-strength microjet under low temperature
Homogenization, micro-nano cellulose is obtained after freeze-drying.But this method reaction time is long, efficiency is low, and general enzyme compares
Expensive and condition is relatively harsh.
The content of the invention
The present invention provides one kind using plant fiber as raw material, micro nanometer fiber is prepared with reference to Physical and chemical method
Element, the micro-nano cellulose good dispersion prepared with this method, stability are high, size uniform；And this method is easy to operate, into
This is relatively low, and spent acid can reuse, and reduce environmental pollution, be adapted for carrying out industrialized production.
A kind of preparation method of micro-nano cellulose described in the present invention, includes the following steps：
1) plant fiber is crushed with pulverizer, crosses 40 mesh and 100 mesh sieves, take the fiber dust of center section；
2) it is NaOH solution that fiber dust is 2%~5% with mass fraction by 1g/20mL~1g/30mL by solid-to-liquid ratio
1h~2h is pre-processed under the conditions of 70 DEG C~80 DEG C, it is therefore an objective to wash away impurity and dissolved lignin；
3) pretreated fiber dust is filtered out, it is dry after washing to neutrality；
4) be 1g/20mL~1g/30mL by solid-to-liquid ratio, by pretreated fiber dust mass fraction for 40%~
60% inorganic acid stirring hydrolysis 1h~3h, hydrolysis temperature is 40 DEG C~60 DEG C, then adds 1/3~2/3 times of deionized water,
Terminate hydrolysis；
5) suspension of the micro-nano cellulose acid after hydrolysis is separated and collected into spent acid and micro-nano cellulose dope；
6) it is anti-after micro-nano cellulose dope being neutralized to neutrality with NaOH solution in 1/2~1 times of deionized water
Centrifugation 2-3 times is washed in after backwashing, or is washed in sand core funnel with excessive deionized water to neutrality；
7) it will wash to neutral micro-nano cellulose dope and be freeze-dried, up to micro-nano cellulose.
Above-mentioned described plant fiber material can be bamboo fiber, bamboo pulp fiber, sawdust, bagasse, stalk, peanut shell
Deng.
Inorganic acid described in above-mentioned steps 4 can be H2SO4Or HCl or H2SO4With the mixed liquor of HCl, H2SO4:HCl=5:
1~3:1.
This method prepare micro-nano cellulose odorlessness, tasteless, not soluble in water and organic solvent, particle diameter 50 μm with
It is interior, it is corynebacterium, and micro-nano cellulose good dispersion, stability height, yield reach as high as institute in 71.4% and preparation process
The spent acid of generation can reuse after simple process, reduce the pollution to environment；Whole preparation process is easy to operate, into
This is low, and energy consumption is low.
Brief description of the drawings:
Fig. 1 is the scanning electron microscope (SEM) photograph of micro-nano cellulose made from embodiment 1.
Fig. 2 is the grain size distribution of micro-nano cellulose in supernatant in embodiment 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of micro-nano cellulose made from embodiment 2.
Fig. 4 is the scanning electron microscope (SEM) photograph of micro-nano cellulose made from embodiment 5.
Fig. 5 is the scanning electron microscope (SEM) photograph of micro-nano cellulose made from embodiment 6.
Fig. 6 is the scanning electron microscope (SEM) photograph of micro-nano cellulose made from embodiment 7.
Embodiment
Embodiment 1
Take 20g bamboo fibers to be crushed with pulverizer, cross 40 mesh and 100 mesh sieves, take the fiber dust of center section.By fiber
Powder pre-processes 1.5h with the NaOH solution that 400ml mass fractions are 3% under the conditions of 70 DEG C, washes away impurity and dissolves wooden
Element, after treatment filtering, dry 12h after being washed with deionized to neutrality.Then the pretreated fiber powders of wherein 3g are taken
End, is put into 100mL three-necked flasks；The H that 60mL mass fractions are 50% is added into flask2SO4Solution, water under the conditions of 50 DEG C
Solve 2h.20mL deionized waters are added after hydrolysis and terminate reaction, are cooled to room temperature.Mixed liquor after hydrolysis is poured into centrifuge tube
In centrifuge 10min under 1000rpm.Dope after centrifugation is placed in beaker, 60mL deionized waters is added, uses NaOH solution
It is neutralized to pH=7.Then centrifuge, wash, centrifuge again again, in triplicate.It is dry by freezing by obtained dope is finally centrifuged
It is dry, that is, obtain micro-nano cellulose, yield 71.4%.
Obtained micro-nano cellulose is observed with HITACHI S-4800 scanning electron microscope, can from Fig. 1
The micro-nano cellulose prepared using finding out is corynebacterium, and granularity is within 50 μm.Obtained micro-nano cellulose is dispersed in
In water, stood after being ultrasonically treated 10min, take its supernatant after largely precipitating, swashed with Malvern Nano ZS type Malverns
Light particle size analyzer detects its supernatant size distribution, and as can be seen from Figure 2 the particle diameter of cellulose is evenly distributed in supernatant
300nm or so, the micro-nano cellulose for illustrating to prepare also have in addition to the cellulose for the part micron level that electron microscopic observation goes out
There are the cellulose of part Nano grade.
Embodiment 2
Take 20g bamboo fibers to be crushed with pulverizer, cross 40 mesh and 100 mesh sieves, take the fiber dust of center section.By fiber
Powder pre-processes 1.5h with the NaOH solution that 450ml mass fractions are 3% under the conditions of 70 DEG C, washes away impurity and dissolves wooden
Element, after treatment filtering, dry 12h after being washed with deionized to neutrality.Then the pretreated fiber powders of wherein 3g are taken
End, is put into 100mL three-necked flasks；60mL mass fractions are added into flask as 50% HCl solution, ultrasound under the conditions of 50 DEG C
Hydrolysis process 1.5h.After add 20mL deionized waters and terminate reaction, be cooled to room temperature.By the mixed liquor after hydrolysis pour into from
In the heart pipe 10min is centrifuged under 1000rpm.Dope after centrifugation is placed in beaker, 60mL deionized waters is added, uses NaOH
Solution is neutralized to pH=7.Then centrifuge, wash, centrifuge again again, in triplicate.Obtained dope will finally be centrifuged through supercooling
It is lyophilized dry, that is, obtain micro-nano cellulose, yield 69.8%.
As can be seen from Figure 3 the micro-nano cellulose prepared and particle diameter and shape characteristic in embodiment 1 are basically identical,
Illustrate that ultrasonic wave added can promote hydrolysis well, improve hydrolysis efficiency.
Embodiment 3
The pretreatment of bamboo fiber with embodiment 1, take the pretreated fiber dusts of 3g, be put into 100mL three-necked flasks
In；Acid solution (the m that 60mL mass fractions are 50% is added into flaskH2SO4:mHCl=4:1), 2h is hydrolyzed under the conditions of 50 DEG C.Hydrolysis
After add 20mL deionized waters and terminate reaction, be cooled to room temperature.By the mixed liquor after hydrolysis pour into centrifuge tube
10min is centrifuged under 1000rpm.Dope after centrifugation is placed in beaker, 60mL deionized waters is added, is neutralized with NaOH solution
To pH=7.Then centrifuge, wash, centrifuge again again, in triplicate.Obtained dope will finally be centrifuged by being freeze-dried, i.e.,
Obtain micro-nano cellulose, yield 70.9%.
Embodiment 4
With 3% NaOH solution, its concentration A=7.5 × 10-4Mol/g, using phenolphthalein as indicator, is dripped with the NaOH solution
Determine the spent acid produced in 1g embodiments 1, consumption NaOH solution quality mA=9.87g, calculate spent acid concentration B=1/2A × mA
=3.7 × 10-3The mass fraction B of moL/g, then spent acid1=98B=36.3%.Then 50% is configured with spent acid and the concentrated sulfuric acid
H2SO4, the quality 100g of spent acid is taken, then the quality for needing the concentrated sulfuric acid is Y=(0.5-B1) × 100/0.48=28.54g.
The pretreatment of bamboo fiber takes the pretreated fiber dusts of 3g, is put into 100mL three-necked flasks with embodiment 1；
50% H that 60mL is prepared again with spent acid is added into flask2SO4Solution, hydrolyzes 2h under the conditions of 50 DEG C.Add after hydrolysis
Enter 20mL deionized waters and terminate reaction, be cooled to room temperature.Mixed liquor after hydrolysis is poured into centrifuge tube and is centrifuged under 1000rpm
10min.Dope after centrifugation is placed in beaker, 60mL deionized waters is added, pH=7 is neutralized to NaOH solution.Then
Centrifuge, wash, centrifuge again again, in triplicate.Obtained dope will finally be centrifuged by freeze-drying, that is, obtain micro-nano fibre
Dimension element, yield 69%.
As can be seen from Figure 4：The micro-nano cellulose particle diameter prepared is corynebacterium within 30 μm, is illustrated with useless
The acid solution that acid and the concentrated sulfuric acid are prepared can continue, for preparing micro-nano cellulose, not only to economize on resources, also reduce environment dirt
Dye.
Embodiment 5
Take 20g bamboo pulp fibers to be crushed with pulverizer, cross 40 mesh and 100 mesh sieves, take the fiber dust of center section.By fiber
Powder pre-processes 1.5h with the NaOH solution that 450ml mass fractions are 3% under the conditions of 70 DEG C, washes away impurity and dissolves wooden
Element, after treatment filtering, dry 12h after being washed with deionized to neutrality.Then the pretreated fiber powders of wherein 3g are taken
End, is put into 100mL three-necked flasks；The H that 60mL mass fractions are 50% is added into flask2SO4Solution, water under the conditions of 50 DEG C
Solve 2h.20mL deionized waters are added after hydrolysis and terminate reaction, are cooled to room temperature.Mixed liquor after hydrolysis is poured into centrifuge tube
In centrifuge 10min under 1000rpm.Dope after centrifugation is placed in beaker, 60mL deionized waters is added, uses NaOH solution
It is neutralized to pH=7.Then centrifuge, wash, centrifuge again again, in triplicate.It is dry by freezing by obtained dope is finally centrifuged
It is dry, that is, obtain micro-nano cellulose, yield 63.7%.
As can be seen from Figure 5 at 50 μm or so, a part is in the form of a column the micro-nano cellulose particle diameter prepared, a part
In the form of sheets.
Embodiment 6
Take 20g sawdusts to be crushed with pulverizer, cross 40 mesh and 100 mesh sieves, take the powder of center section.By powder 400ml
The NaOH solution that mass fraction is 3% pre-processes 1.5h under the conditions of 70 DEG C, washes away impurity and dissolved lignin, after treatment
Filtering, dry 12h after being washed with deionized to neutrality.Then the pretreated powder of wherein 2g is taken, is put into tri- mouthfuls of burnings of 100mL
In bottle；The H that 50mL mass fractions are 50% is added into flask2SO4Solution, hydrolyzes 2h under the conditions of 50 DEG C.Added after hydrolysis
20mL deionized waters terminate reaction, are cooled to room temperature.Mixed liquor after hydrolysis is filtered with sand core funnel, is washed to neutrality, will
The dope being finally obtained by filtration obtains micro-nano cellulose, yield 56.2% by freeze-drying.
As can be seen from Figure 6：The micro-nano cellulose particle diameter prepared is in the form of a column within 60 μm, fiber surface ratio
Rougher, surrounding impurities are more, illustrate that content of cellulose is relatively low in sawdust.
Embodiment 7
Plant fiber raw material are changed to peanut shell, remaining step passes through the dope being finally obtained by filtration with embodiment 6
Freeze-drying is crossed, that is, obtains micro-nano cellulose, yield 63.3%.
Embodiment 8
Take 20g stalks to be crushed with pulverizer, cross 40 mesh and 100 mesh sieves, take the powder of center section.By powder 400ml
The NaOH solution that mass fraction is 3% pre-processes 1.5h under the conditions of 70 DEG C, washes away impurity and dissolved lignin, after treatment
Filtering, dry 12h after being washed with deionized to neutrality.Then the pretreated powder of wherein 2g is taken, is put into tri- mouthfuls of burnings of 100mL
In bottle；The H that 50mL mass fractions are 50% is added into flask2SO4Solution, hydrolyzes 2h under the conditions of 50 DEG C.Added after hydrolysis
20mL deionized waters terminate reaction, are cooled to room temperature.Mixed liquor after hydrolysis is filtered with sand core funnel, is washed to neutrality, will
The dope being finally obtained by filtration obtains micro-nano cellulose, yield 50.7% by freeze-drying.
Embodiment 9
Plant fiber raw material are changed to bagasse, remaining step passes through the dope being finally obtained by filtration with embodiment 8
Freeze-drying, that is, obtain micro-nano cellulose, yield 38.3%.
Claims (3)
1. a kind of preparation method of micro-nano cellulose, it is characterised in that comprise the following steps that：
1) plant fiber is crushed with pulverizer, crosses 40 mesh and 100 mesh sieves, take the fiber dust of center section；
2) by solid-to-liquid ratio be 1g/20mL~1g/30mL by fiber dust be 2%~5% with mass fraction NaOH solution 70
DEG C~80 DEG C under the conditions of pre-process 1h~2h；
3) pretreated fiber dust is filtered out, it is dry after washing to neutrality；
4) it is 1g/20mL~1g/30mL by solid-to-liquid ratio, is 40%~60% by pretreated fiber dust mass fraction
Inorganic acid stirring hydrolysis 1h~3h, hydrolysis temperature is 40 DEG C~60 DEG C, then adds 1/3~2/3 times of deionized water, terminates water
Solution reaction；
5) suspension of the micro-nano cellulose acid after hydrolysis is separated and collected into spent acid and micro-nano cellulose dope；
6) washed repeatedly after micro-nano cellulose dope being neutralized to neutrality with NaOH solution in 1/2~1 times of deionized water
Centrifugation 2-3 times is washed, or is washed in sand core funnel with excessive deionized water to neutrality；
7) it will wash to neutral micro-nano cellulose dope and be freeze-dried, up to micro-nano cellulose.
2. a kind of preparation method of micro-nano cellulose as claimed in claim 1, it is characterised in that above-mentioned described plant is fine
It can be bamboo fiber, bamboo pulp fiber, sawdust, bagasse, stalk, peanut shell etc. to tie up raw material.
A kind of 3. preparation method of micro-nano cellulose as claimed in claim 1, it is characterised in that the nothing described in above-mentioned steps 4
Machine acid can be H2SO4Or HCl or H2SO4With the mixed liquor of HCl, H2SO4:HCl=5:1~3:1.
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| CN108892221A (en) * | 2018-06-21 | 2018-11-27 | 湖南双晟科技信息咨询有限公司 | A method of water body fluoride removal material is prepared using solid waste |
| WO2019196373A1 (en) * | 2018-04-10 | 2019-10-17 | 华南理工大学 | Method for separating cellulose by grade by using microchannel |
| CN110863385A (en) * | 2019-11-28 | 2020-03-06 | 广西科技师范学院 | Method for preparing high-concentration microfibrillated cellulose dispersion |
| CN112159648A (en) * | 2020-09-04 | 2021-01-01 | 厦门大学 | Preparation method of drilling fluid filtrate reducer |
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| CN113929821A (en) * | 2021-10-28 | 2022-01-14 | 西南石油大学 | Preparation method of nano-cellulose derivative with good performance |
| CN114534502A (en) * | 2022-02-14 | 2022-05-27 | 天津大学 | CNC hydrolysis acid circulation process based on diffusion dialysis and electrodialysis series combination |
| CN114534503A (en) * | 2022-02-14 | 2022-05-27 | 天津大学 | Continuous separation and recovery device and method for high-concentration waste acid applied to CNC (computerized numerical control) production |
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| CN114534502A (en) * | 2022-02-14 | 2022-05-27 | 天津大学 | CNC hydrolysis acid circulation process based on diffusion dialysis and electrodialysis series combination |
| CN114534503A (en) * | 2022-02-14 | 2022-05-27 | 天津大学 | Continuous separation and recovery device and method for high-concentration waste acid applied to CNC (computerized numerical control) production |
| CN114534500A (en) * | 2022-02-14 | 2022-05-27 | 天津大学 | Low-concentration waste acid separation and recovery device and method applied to CNC production |
| CN115012052A (en) * | 2022-04-29 | 2022-09-06 | 北华大学 | Method for preparing micro-nano cellulose fibers by taking corn straws as raw materials |
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