CN107245766A - A kind of cellulose nano-fibrous preparation method of low energy consumption - Google Patents
A kind of cellulose nano-fibrous preparation method of low energy consumption Download PDFInfo
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- CN107245766A CN107245766A CN201710534501.1A CN201710534501A CN107245766A CN 107245766 A CN107245766 A CN 107245766A CN 201710534501 A CN201710534501 A CN 201710534501A CN 107245766 A CN107245766 A CN 107245766A
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
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Abstract
The invention discloses a kind of cellulose nano-fibrous preparation method of low energy consumption, after dry cellulosic material is sufficiently stirred for into swollen in tetrabutylammonium acetate ammonium and dimethyl sulfoxide (DMSO) mixed solution, add maleic anhydride, through centrifuge washing after reacting in a mild condition, by the obtained cellulose nano-fibrous cellulose nano-fibrous aqueous dispersions for shifting in water, being stablized.This method need not move through any type of mechanical treatment just can with a step handle be uniformly dispersed, size uniformity it is cellulose nano-fibrous.The diameter of fiber is evenly distributed, about 5 10nm, length>500nm.The method that the present invention is provided effectively can be made cellulose nano-fibrous by the step of bamboo wood dissolving pulp one, and technological operation is easy, and energy consumption is low, it is possible to complete to be modified the surface of cellulose simultaneously during preparation, there is wide prospect in application aspect.
Description
Technical field
The invention belongs to natural macromolecular material field, and in particular to a kind of cellulose nano-fibrous preparation of low energy consumption
Method.
Background technology
In recent years, as people understand in depth to green living and environmental protection, everybody is to degradable green product
Demand is growing day by day.Cellulose also receives people and more and more paid close attention to as a kind of biodegradable material.It is used as generation
Content the abundantest natural polymer in boundary, nature can synthesize about 100,000,000,000 tons of cellulose every year, and it is recyclable again
It is raw.Due to the hydrogen bond action existed between native cellulose molecule so that cellulose generate powerful hydrogen bond network structure, compared with
High molecular weight and crystallinity, but due to its supramolecular structure, be difficult to dissolve cellulose in common solvent, its melting temperature connects
Its nearly decomposition temperature, thus largely limit its application.In nano-scale range control cellulosic molecule and
Its supramolecular aggregation, and the new nanometer fine chemical product with excellent function, new nano material are thus createed, as fiber
The Disciplinary Frontiers of plain science.Compared to powder cellulose and microcrystalline cellulose, cellulose nano-fibrous (cellulose
Nanofibers, CNF) there are many excellent performances, such as high transparency, high-crystallinity, high-purity, high Young's modulus, hyperfine
Structure, high polymerization degree, high-hydrophilic and high intensity etc..Therefore, the research of cellulose nano-fibrous preparation and application is state
The emphasis and focus of inside and outside cellulose chemistry research.
Although having been developed for many methods for preparing cellulose nano-fibrous material, such as physicomechanical processes at present
(CN102220718A, CN103492637A), TEMPO oxidation (CN103827146A, Biomacromolecules, 2006,
7,1687) method such as, but because these methods or high energy consumption or the problem of there is pollution environment so that cellulose is received
Rice fiber large batch of can not be produced and applied.
Ionic liquid at room temperature can dissolve gas chromatography and inorganic matter and can be recycled, environmentally friendly as one kind
Green solvent, it is just progressively applied to cellulose nano-fibrous preparation.Since 1970, some organic solvent systems are
Develop for directly dissolving cellulose, such as dimethyl acetamide-lithium chloride mixed system (DMAc-LiCl) (US, 1980;
Cellulose, 2003,10,283) N-methyl morpholine oxide-water mixed system (NMMO-H2O) (Progress
in Polymer Science, 2001, 26, 1473; ActaPolytechnicaHungarica, 2008, 5;
Cellulose, 2002,9,283), equal solvent system.Solubility of the cellulose in DMAc-LiCl is very low, so it
Business application is limited.Cellulose is in NMMO-H2There is higher solvability in O, and applied to cellulose fibre
Industrialized production.This process is a closed-loop system and NMMO can be reclaimed, therefore it is generally acknowledged a kind of environment-friendly
The method for preparing cellulose fibre.However, NMMO and cellulose have the trend of decomposition under harsher dissolution conditions
(Cellulose, 2002, 9, 283; Holzforschung, 2001, 55, 661)。
In recent years, ion liquid of quaternaries, such as tetrabutyl ammonium fluoride (TBAF) (Macromolecular
Chemistry ＆ Physics, 2000,201,627), etamon chloride (TEAC), 40% TBAH
(TBAH) it is found to can be used for dissolving cellulose and there is higher solvability (Chemical with cosolvent
Communications, 2012, 48, 1808).For TBAF and TEAC, DMSO is a kind of excellent cosolvent
(Journal of Polymer Science Polymer Symposia, 1973, 42, 1531)；And DMSO is a kind of
Excellent polymer sweller (Biomacromolecules, 2009,10,2401).
Regulatable dissolving is carried out to cellulosic material using the synergy of ion liquid of quaternaries and cosolvent,
Developed on the basis of this it is a kind of prepare cellulose nano-fibrous method, the energy consumption in preparation process can be effectively reduced, prepare
Go out size uniform, it is stable cellulose nano-fibrous.
The content of the invention
Goal of the invention：Present invention aims at a kind of cellulose nano-fibrous preparation method of low energy consumption is provided, effectively
Prepare and be uniformly dispersed, controllable single cellulose nano-fibrous of size uniformity.
Technical scheme：In order to realize foregoing invention purpose, the technical solution adopted by the present invention is：
A kind of cellulose nano-fibrous preparation method of low energy consumption, it comprises the following steps：
1）Raising is carried out to cellulosic material, is disperseed；
2）Cellulosic material after first will be scattered carries out swollen in ionic liquid, and then acid anhydrides is directly added into ionic liquid
Reacted；
3）With dimethyl sulfoxide (DMSO) to step 2）Middle fiber is washed, centrifugation, removes ionic liquid and unreacted acid anhydrides, obtains steady
Fixed cellulose nano-fibrous suspension；
4）By step 3）The cellulose nano-fibrous element of gained is dispersed in organic solvent, or is redispersed in by alcohol solvent displacement
In water, the water slurry stablized.
The cellulose nano-fibrous preparation method of described low energy consumption, swollen temperature is 30 DEG C, and the time is 30min-2h.
The cellulose nano-fibrous preparation method of described low energy consumption, acid anhydrides used is maleic anhydride or succinic anhydride.
In the cellulose nano-fibrous preparation method of described low energy consumption, cellulose and anhydride reaction, acid anhydrides and dehydration Portugal
The mol ratio of grape sugar is 2-25:1.
In the cellulose nano-fibrous preparation method of described low energy consumption, cellulose and anhydride reaction, reaction temperature is 30
DEG C, the reaction time is 30min-1h.
The cellulose nano-fibrous preparation method of described low energy consumption, organic solvent includes dimethyl sulfoxide (DMSO), N, N- diformazans
Base formamide, DMA.
Step 1）In, detailed process is：Cellulosic material is discongested using PTI and PFI mills, the raw material warp after discongesting
Cross and dry, then disperse 5min with IKA grinder and obtain fluffy cellulosic material；Concrete operations condition：Existed with PTI mills
Discongest 10min under 15000rpm, after under 1000rpm-3000rpm discongest 10min with PFI mills.
Step 2）In, it is specially：Use TBAA concentration former to cellulose for 1%-5% TBAA/DMSO ion liquid systems
Material swelling treatment 1h at 30 DEG C, is subsequently added the acid anhydrides of different proportion and is reacted under preference temperature.
Step 3）In, it is specially：Centrifugal treating：The above-mentioned cellulose ionic liquid mixture after anhydride reaction is through diformazan
After sulfoxide washing under 12500 rpm, 10min is centrifuged, supernatant is removed, takes Cellulose precipitates, finally give stable dispersion
Cellulose nano-fibrous solution.
Beneficial effect：Compared with prior art, advantages of the present invention includes：
1）Energy consumption needed for preparation process of the present invention is overall is low, and cellulosic material is by being swelled, it is any to need not move through after anhydride reaction
The cellulose nano-fibrous of size uniform can be made in mechanical treatment, be it is existing prepare it is cellulose nano-fibrous（CNF）In technology
It is unexistent, it is the breakthrough to prior art.
2）Reaction is in room temperature in the present invention, and mild condition is easy to control.
3）Substitution value different cellulose nano-fibrous in surface can be obtained by the ratio for regulating and controlling to add acid anhydrides；Obtain
Substitution value higher cellulose nano-fibrous in surface is easy in water form gel, with preferable application prospect.
4）Cellulose nano-fibrous size uniform produced by the present invention, draw ratio is larger, and fibre diameter is about 5-10nm, long
Degree is more than 500 nm.
5）The present invention solves existing chemical method and Physical, and strong acid corrosivity is strong, and equipment requirement is high, and energy consumption is big, with
And obtained cellulose nano-fibrous size is uneven, between fiber easily aggregation the problems such as, the present invention is easy to operate, efficiently
And modified cellulose nano-fibrous in surface can be directly obtained.
Brief description of the drawings
Fig. 1 is transmission electron microscope figure cellulose nano-fibrous made from embodiment 1；
Fig. 2 is transmission electron microscope figure cellulose nano-fibrous made from embodiment 2；
Fig. 3 is transmission electron microscope figure cellulose nano-fibrous made from embodiment 3；
Fig. 4 is raw material bamboo wood dissolving pulp and obtained cellulose nano-fibrous x-ray diffraction pattern used.
Embodiment
Illustrate present disclosure with reference to instantiation.It should be understood that these examples be merely to illustrate the present invention and
It is not used in limitation the scope of the present invention.Furthermore, it is to be understood that after the content of the invention lectured has been read, those skilled in the art
The present invention can be made various changes or modifications, these equivalent form of values equally fall within what the application appended claims were limited
Scope.
Embodiment 1
Bamboo wood dissolving pulpboard is ground with PTI and under 15000rpm discongests 10min, after dredged with PFI mills under 1000rpm-3000rpm
Solve 10min；Pulpboard after discongesting passes through drying, then obtains fluffy cellulosic material with the scattered 5min of IKA grinder.Take
0.1g it is above-mentioned it is scattered after bamboo wood dissolving pulp add 10g TBAA concentration in 3% TBAA/DMSO ion liquid systems, 30 DEG C
Under be swelled 1h.Then, it is 25 mol ratio to be added immediately:1 maleic anhydride, reacts 60min at 65 DEG C.Finally plus DMSO washing,
10min is centrifuged under 12500rpm, supernatant is removed, it is repeated multiple times until obtaining the cellulose nano-fibrous of white；Again plus ethanol
Centrifugation removes supernatant, washes twice；Centrifugation finally add water once, cellulose nano-fibrous hydrogel is obtained.
Embodiment 2
Bamboo wood dissolving pulpboard is ground with PTI and under 15000rpm discongests 10min, after dredged with PFI mills under 1000rpm-3000rpm
Solve 10min；Pulpboard after discongesting passes through drying, then obtains fluffy cellulosic material with the scattered 5min of IKA grinder.Take
0.1g it is above-mentioned it is scattered after bamboo wood dissolving pulp add 10g TBAA concentration in 3% TBAA/DMSO ion liquid systems, 30 DEG C
Lower swollen 1h.Then, it is 8 mol ratio to be added immediately:1 maleic anhydride, reacts 30min at 60 DEG C.Finally plus DMSO washing,
10 min are centrifuged under 12500 rpm, supernatant is removed, it is repeated multiple times until obtaining the cellulose nano-fibrous of white；Again plus second
Alcohol centrifugation removes supernatant, washes twice；Centrifugation finally add water once, cellulose nano-fibrous hydrogel is obtained.
Embodiment 3
Bamboo wood dissolving pulpboard is ground with PTI and under 15000rpm discongests 10min, after dredged with PFI mills under 1000rpm-3000rpm
Solve 10min；Pulpboard after discongesting passes through drying, then obtains fluffy cellulosic material with the scattered 5min of IKA grinder.Take
0.1g it is above-mentioned it is scattered after bamboo wood dissolving pulp add 10g TBAA concentration in 3% TBAA/DMSO ion liquid systems, 30 DEG C
Lower swollen 1h.Then, it is 8 mol ratio to be added immediately:1 maleic anhydride, reacts 30 min at 30 DEG C.Finally plus DMSO, 12500
10 min are centrifuged under rpm, supernatant is removed, it is repeated multiple times until obtaining the cellulose nano-fibrous of white；Again plus ethanol centrifugation
Supernatant is removed, is washed twice；Centrifugation finally add water once, cellulose nano-fibrous hydrogel is obtained.
Embodiment 4
Bamboo wood dissolving pulpboard is ground with PTI and under 15000rpm discongests 10min, after dredged with PFI mills under 1000rpm-3000rpm
Solve 10min；Pulpboard after discongesting passes through drying, then obtains fluffy cellulosic material with the scattered 5min of IKA grinder.Take
0.1g it is above-mentioned it is scattered after bamboo wood dissolving pulp add 10g TBAA concentration in 3% TBAA/DMSO ion liquid systems, 30 DEG C
Lower swollen 1h.Then, it is 6 mol ratio to be added immediately:1 maleic anhydride, reacts 30min at 30 DEG C.Finally plus DMSO, 12500
10 min are centrifuged under rpm, supernatant is removed, it is repeated multiple times until obtaining the cellulose nano-fibrous of white；Again plus ethanol centrifugation
Supernatant is removed, is washed twice；Centrifugation finally add water once, cellulose nano-fibrous hydrogel is obtained.
Embodiment 5
Bamboo wood dissolving pulpboard is ground with PTI and under 15000rpm discongests 10min, after dredged with PFI mills under 1000rpm-3000rpm
Solve 10min；Pulpboard after discongesting passes through drying, then obtains fluffy cellulosic material with the scattered 5min of IKA grinder.Take
0.1g it is above-mentioned it is scattered after bamboo wood dissolving pulp add 10g TBAA concentration in 2% TBAA/DMSO ion liquid systems, 30 DEG C
Lower swollen 1h.Then, it is 6 mol ratio to be added immediately:1 maleic anhydride, reacts 30min at 60 DEG C.Finally plus DMSO, 12500
10 min are centrifuged under rpm, supernatant is removed, it is repeated multiple times until obtaining the cellulose nano-fibrous of white；Again plus ethanol centrifugation
Supernatant is removed, is washed twice；Centrifugation finally add water once, cellulose nano-fibrous hydrogel is obtained.
Embodiment 6
Bamboo wood dissolving pulpboard is ground with PTI and under 15000rpm discongests 10min, after dredged with PFI mills under 1000rpm-3000rpm
Solve 10min；Pulpboard after discongesting passes through drying, then obtains fluffy cellulosic material with the scattered 5min of IKA grinder.Take
0.1g it is above-mentioned it is scattered after bamboo wood dissolving pulp add 10g TBAA concentration in 3% TBAA/DMSO ion liquid systems, 30 DEG C
Lower swollen 1h.Then, it is 4 mol ratio to be added immediately:1 succinic anhydride, reacts 30min at 30 DEG C.Finally plus DMSO, 12500
10 min are centrifuged under rpm, supernatant is removed, it is repeated multiple times until obtaining the cellulose nano-fibrous of white；Again plus ethanol centrifugation
Supernatant is removed, is washed twice；Centrifugation finally add water once, cellulose nano-fibrous hydrogel is obtained.
Referring to accompanying drawing, TEM detections are carried out respectively to the cellulose nano-fibrous of the preparation of embodiment 1,2,3, as a result shown
Prepare it is cellulose nano-fibrous be single fiber, and be uniformly dispersed, size uniformity.Diameter is between 5-10nm.
Claims (10)
1. a kind of cellulose nano-fibrous preparation method of low energy consumption, it comprises the following steps：
1）Raising, decentralized processing are carried out to dry cellulosic material；
2）Cellulosic material after first will be scattered carries out swollen in ionic liquid, and then acid anhydrides is directly added into ionic liquid
Reacted；
3）With dimethyl sulfoxide (DMSO) to step 2）Middle fiber is washed, centrifugation, removes ionic liquid and unreacted acid anhydrides, obtains steady
Fixed cellulose nano-fibrous suspension；
4）By step 3）The cellulose nano-fibrous element of gained is dispersed in organic solvent, or is redispersed in by alcohol solvent displacement
In water, the water slurry stablized.
2. the cellulose nano-fibrous preparation method of described low energy consumption is required according to right 1, it is characterised in that：Used from
Sub- liquid is tetrabutylammonium acetate ammonium, and cosolvent is dimethyl sulfoxide (DMSO).
3. the cellulose nano-fibrous preparation method of described low energy consumption is required according to right 1, it is characterised in that：Swollen temperature is
30 ~ 65 DEG C, the time is 30min-2h.
4. the cellulose nano-fibrous preparation method of described low energy consumption is required according to right 1, it is characterised in that：Acid anhydrides used is
Maleic anhydride or succinic anhydride.
5. the cellulose nano-fibrous preparation method of described low energy consumption is required according to right 1, it is characterised in that：Cellulose and acid
In anhydride reactant, the mol ratio of acid anhydrides and dehydrated glucose is 2-25:1.
6. the cellulose nano-fibrous preparation method of described low energy consumption is required according to right 1, it is characterised in that：Cellulose and acid
In anhydride reactant, reaction temperature is 30 ~ 65 DEG C, and the reaction time is 30min-1h.
7. the cellulose nano-fibrous preparation method of described low energy consumption is required according to right 1, it is characterised in that：Organic solvent bag
Include dimethyl sulfoxide (DMSO), DMF, DMA.
8. the cellulose nano-fibrous preparation method of described low energy consumption is required according to right 1, it is characterised in that：Step 1）In,
Detailed process is：Cellulosic material is discongested using PTI and PFI mills, the raw material after discongesting passes through drying, then is ground with IKA
Grinding machine（A10 basic）Scattered 5min obtains fluffy cellulosic material.
9. the cellulose nano-fibrous preparation method of described low energy consumption is required according to right 1, it is characterised in that：Step 2）In,
Specially：Use TBAA concentration for 1%-5% TBAA/DMSO ion liquid systems to the cellulosic material after scattered at 30 DEG C
Swelling treatment 1h, is subsequently added the acid anhydrides of different proportion and is reacted under preference temperature.
10. the cellulose nano-fibrous preparation method of described low energy consumption is required according to right 1, it is characterised in that：Step 3）In,
Specially：Centrifugal treating：It is above-mentioned after cellulose ionic liquid mixture is washed through dimethyl sulfoxide after anhydride reaction 12500
Under rpm, 10min is centrifuged, supernatant is removed, takes Cellulose precipitates, finally give the cellulose nano-fibrous solution of stable dispersion.
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Cited By (6)
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| CN108822320A (en) * | 2018-07-10 | 2018-11-16 | 南京林业大学 | A method of modified cellulose and UV-resistant thin film is prepared in ionic liquid at room temperature |
| CN108997596A (en) * | 2018-07-09 | 2018-12-14 | 南京林业大学 | A method of from preparing reuse ionic liquid in cellulose nano-fibrous waste liquid |
| WO2019105287A1 (en) * | 2017-12-01 | 2019-06-06 | 济南圣泉集团股份有限公司 | Nanocellulose, preparation method therefor and use thereof |
| CN109970875A (en) * | 2019-04-12 | 2019-07-05 | 四川大学 | It is a kind of cellulose nano-fibrous and preparation method thereof |
| CN113123159A (en) * | 2021-04-09 | 2021-07-16 | 陕西科技大学 | Cellulose nano fibril suspension and preparation method thereof |
| CN113668084A (en) * | 2021-08-12 | 2021-11-19 | 武汉大学 | Cellulose nanofiber and preparation method thereof |
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| CN108997596B (en) * | 2018-07-09 | 2020-12-15 | 南京林业大学 | Method for recycling ionic liquid from waste liquid for preparing cellulose nano-fibers |
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| CN109970875A (en) * | 2019-04-12 | 2019-07-05 | 四川大学 | It is a kind of cellulose nano-fibrous and preparation method thereof |
| CN113123159A (en) * | 2021-04-09 | 2021-07-16 | 陕西科技大学 | Cellulose nano fibril suspension and preparation method thereof |
| CN113668084A (en) * | 2021-08-12 | 2021-11-19 | 武汉大学 | Cellulose nanofiber and preparation method thereof |
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