CN108221438A - A kind of preparation method of bleached eucalyptus pulp nano-cellulose - Google Patents
A kind of preparation method of bleached eucalyptus pulp nano-cellulose Download PDFInfo
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- CN108221438A CN108221438A CN201711288612.5A CN201711288612A CN108221438A CN 108221438 A CN108221438 A CN 108221438A CN 201711288612 A CN201711288612 A CN 201711288612A CN 108221438 A CN108221438 A CN 108221438A
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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
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/001—Modification of pulp properties
- D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
- D21C9/004—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives inorganic compounds
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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
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/001—Modification of pulp properties
- D21C9/007—Modification of pulp properties by mechanical or physical means
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- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of preparation methods of bleached eucalyptus pulp nano-cellulose, belong to nano-cellulose preparation field.This method is：Bleached eucalyptus pulp is impregnated, then blended and slurry is obtained by filtration using NaOH prepreg solutions；Slurry is mixed with ammonium persulfate solution, heating stirring is reacted under the conditions of 80 DEG C of water-bath；After the reaction was complete, centrifuge washing adjusts pH, under the conditions of 70 DEG C, adds in H2O2Carry out ultrasound；It is centrifuged after reaction, adjusts pH to neutrality, ultrasonic disperse obtains nano-cellulose suspension.Nano-cellulose dispersibility prepared by this method, stability is preferable, and yield is higher, and need not consume a large amount of acid solutions, can prepare nanocomposite and applied to fields such as food, papermaking, biological medicine and cosmetics as ideal functional filler.
Description
Technical field
The invention belongs to nano-cellulose preparation fields, are related to a kind of preparation method of bleached eucalyptus pulp nano-cellulose.
Background technology
Cellulose is a kind of biological material for being widely present in plant, Some Animals and microorganism, have derive from a wealth of sources,
Characteristic degradable, renewable, at low cost.It is quickly consumed, under the situation of environmental degradation in world today's resource, focusing on exploitation can
Regenerated cellulose and its derivates resource has important strategic importance.Cellulose is prepared into nano material to a certain degree
On solve its present on performance it is insufficient such as：The limitation of not resistant to chemical etching, limited strength etc. and physical aspect, makes this
One renewable resource has broader practice prospect.
Nano-cellulose is derived from a kind of most abundant high polymer of native cellulose, is that cellulose passes through processing, will be fine
The crystal region of amorphous region and low-crystallinity in dimension element is abolished, a kind of cellulose crystallite body extracted.Researcher at present
The nano-celluloses of a variety of separate sources and pattern are made by using various either physically or chemically processing cellulosic materials,
It was found that it not only has light, the degradable characteristic of biological material, while also there is low thermal coefficient of expansion and high surface to react
Property, huge specific surface area, the characteristics such as higher crystallinity and excellent mechanical property, good biodegradability with biology
Compatibility makes it a kind of high molecular nanometer filler of most rich potentiality.
It is effect in various chemical reagent or mechanical force etc. from native cellulose extraction, the principle for preparing nano-cellulose
Under, amorphous region of degrading leaves the higher nanoscale cellulose of crystallinity.At present, nano-cellulose is prepared from biological raw material
Two steps can be divided into：The pretreatment of raw material and the nanosizing of cellulose.The nanosizing of cellulose can be divided into chemical method and machinery at present
Method.Chemical method mainly includes acid hydrolyzation, enzymatic isolation method, oxidizing process etc., and mechanical rule mainly has high-pressure homogeneous, ultrasonic, micro- penetrate
Stream, grinding etc..
Acid hydrolyzation is to prepare the most common method of nano-cellulose, and sour water solution maintains the crystal form of cellulose script.It can
Being used to prepare the inorganic acid of nano-cellulose has sulfuric acid, hydrochloric acid, phosphoric acid and hydrobromic acid etc., and wherein sulfuric acid and hydrochloric acid is more commonly used
Two kinds of inorganic acids.With acid-hydrolyzed continuous application and improvement, sulphuric acid hydrolysis is very ripe now, many factories
Nano cellulose crystal all produced with sulphuric acid hydrolysis, but since sulfuric acid is stronger, consersion unit is required it is high,
It is dangerous big, and residue is difficult recycling in waste liquid, there is certain harm to environment.
Enzymatic isolation method is the selectivity using cellulase, can chance mechanism in the glycosidic bond of cellulose amorphous region, drop
The noncrystalline domain of cellulose is solved, retains crystal region.This method can improve the quality and purity of nano-cellulose, can also reduce soda acid
The dosage of chemicals is waited, reduces water resources consumption and carrying capacity of environment.But enzymatic isolation method is higher to ingredient requirement, needs high-purity
Nano-cellulose raw material, to condition control it is stringenter, cellulosic material need to be pre-processed, and step is comparatively laborious, usually
The nano-cellulose molecular weight of preparation is lower than chemical method.
Mechanical Method is mainly to apply the shearing force or homogeneous of high energy to cellulose, and the fibril between fiber is cut off, from
And the diameter of cellulose is made to be down to Nano grade range, nano-cellulose of the product mostly for threadiness.Mechanical Method prepares nanometer
Cellulose is environmentally safe, but Mechanical Method is the processing to cellulose crystalline region and amorphous region non-selectivity, can destroy portion
Divide crystalline texture, product crystallinity is relatively low.To prepare the preferable nano-cellulose of quality, then need to cellulosic material
Multiple mechanical treatment is carried out, energy consumption is big.
Currently, it is mainly that (2,2,6,6-tetramethyl piperidine oxygen nitrogen is certainly using TEMPO that oxidative degradation, which prepares nano-cellulose,
By base), but contain hypohalite in TEMPO systems, the harmful effect to environment.In recent years scientific research is found, with strong oxygen
The persulfate oxidation plant cellulose for the property changed, can also obtain nano-cellulose.This is mainly due to mistakes under certain condition
Sulfate generates potentiometric titrations and hydrogen peroxide, can be water-soluble micromolecular compound by lignin degradation, and
It can be with the amorphous region in oxidative degradation cellulose, so as to obtain the higher cellulose crystals of crystallinity.
Generally speaking, the method for preparing nano-cellulose that document is reported at present cuts both ways：Acid hydrolyzation is at low cost, effect
Rate is high, but can generate a large amount of spent acid, and danger coefficient is big after reacting；The environmental protection of enzymatic isolation method mild condition, but the general used time is longer, item
Part control is stringenter；To equipment requirement, high, cost increases Physical；Single persulfate system oxidizing process or ultrasonic wave auxiliary
Prepared by the lower oxidative degradation of effect, although simple for process, time-consuming longer, energy consumption, cost are higher.(Wang Xiaoyu, Zhang Yang, river
China waits two methods of to prepare Character Comparison [J] Forestry Engineering journals of nano-cellulose, 2015,29 (6):95-99；
Sun persulfates system prepares research [D] the University Of Agriculture and Forestry In Fujian of carboxylated nano-cellulose and its derivative recklessly,
2014；Cheng M, Qin Z, Liu Y, et al. Efficient extraction of carboxylated
spherical cellulose nanocrystals with narrow distribution through hydrolysis
of lyocell fibers by using ammonium persulfate as an oxidant[J]. Journal of
Materials Chemistry A, 2013, 2(1):251-258；Mascheroni E, Rampazzo R, Ortenzi M
A, et al. Comparison of cellulose nanocrystals obtained by sulfuric acid
hydrolysis and ammonium persulfate, to be used as coating on flexible food-
packaging materials[J]. Cellulose, 2016, 23(1):779-793).Inventor notices persulfate
By generating potentiometric titrations and hydrogen peroxide come the amorphous region in oxidative degradation cellulose.If energy will be to a certain degree
On raw material by persulfate system oxidation pre-treatment, using hydrogen peroxide as individual oxidation system and with combination of ultrasound into
Row processing, accelerated oxidation degradation, it is possible to the reaction time is greatly shortened, yield is high, reduces cost, and product stability is preferable,
The phenomenon that acid hydrolyzation generates a large amount of spent acid, safer environmental protection are avoided simultaneously.
Invention content
It is an object of the invention to be directed to problems of the prior art defect and widen bleached eucalyptus pulp application neck
Domain provides preparation method that is a kind of simple and being easy to industrialized nano-cellulose.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of bleached eucalyptus pulp nano-cellulose, which is characterized in that include the following steps：
(1) bleached eucalyptus pulp in NaOH solution of the mass fraction for 10% ~ 25% is impregnated, obtains prepreg；
(2) prepreg is fully blended, filtration washing obtains slurry；
(3) slurry is uniformly mixed with ammonium persulfate solution, heating stirring is reacted under the conditions of 70 ~ 80 DEG C；
(4) centrifuge washing adds water, adjusts pH to alkalinity；
(5) H is added under the conditions of 60 ~ 70 DEG C2O220 ~ 40 min are stirred by ultrasonic in solution；
(6) centrifuge washing is 6 ~ 8 to pH, and 5 ~ 10 min of ultrasound obtain bleached eucalyptus pulp nano-cellulose suspension.
In the above method, in step (1), the soaking time of the bleached eucalyptus pulp is 5 ~ 10 min.
In the above method, in step (2), the obtained pH of slurry that washs is 6 ~ 8.
In the above method, in step (3), a concentration of 0.8 ~ 1 mol/L of the ammonium persulfate solution, ammonium persulfate
Mass ratio with bleached eucalyptus pulp is 10:1~2.
In the above method, in step (3), the heating reaction time is 2 ~ 3 h.
In the above method, in step (4), the pH is 11 ~ 13.
In the above method, in step (5), the H2O2 The mass fraction of solution is 20% ~ 30%, the H2O2 Solution
Additive amount meet：Step（4）The middle volume and H for adding in water2O2The volume ratio of solution is 40 ~ 50:1.
In the above method, step (6) the bagasse nano-cellulose suspension is water slurry.
In the above method, bagasse nano-cellulose is a diameter of 5 40nm in the bagasse nano-cellulose suspension,
Length is the semicrystalline product of the fibre-like of 100nm 10nm.
It is of the invention compared with existing technology, have the following advantages that：
1st, the preparation method in the present invention is simple and practicable, can be carried from bleached eucalyptus pulp raw material with oxidizing process combination sonic oscillation
Nano-cellulose is taken out, the existing nano-cellulose that prepared from biomass material is avoided and reacts the phenomenon that tediously long complicated, greatly
Shorten reaction time greatly.
2nd, bleached eucalyptus pulp nano-cellulose dispersibility, the stability prepared in the present invention is preferable.
3rd, the reaction reagent used in the present invention is common chemical reagent and reaction condition is mild, at low cost, simultaneously
Bleached eucalyptus pulp utilization ways can be widened, bring higher social value and economic value.Without using acid in reaction process, avoid
It the phenomenon that generation caused by most common strong acid acid hydrolyzation a large amount of spent acid, avoids causing secondary pollution.
4th, the present invention in bleached eucalyptus pulp nano-cellulose preparation method in parameter dosage and preparation condition for
The grain size of the bleached eucalyptus pulp nano-cellulose of gained plays critical influence.
5th, the nano-cellulose being prepared by the method for the present invention can as the raw material for preparing high molecule nano composite material with
And applied in medicine, food and cosmetics.
Description of the drawings
Fig. 1 schemes for bleached eucalyptus pulp nano-cellulose SEM；
Fig. 2 schemes for bleached eucalyptus pulp nano-cellulose FTIR；
Fig. 3 schemes for bleached eucalyptus pulp nano-cellulose TGA.
Specific embodiment
The present invention will be further specifically described in detail with reference to specific embodiments, but embodiments of the present invention are not
It is limited to this, for especially not dated technological parameter, can refer to routine techniques progress.
Embodiment 1
3 g bleached eucalyptus pulps are weighed, 5 min is impregnated for 10% NaOH solution with mass fraction, takes out, blended diafiltration
It washs to pH and obtains slurry for 6 ~ 8.It is uniformly mixed with 300 ml ammonium persulfate solutions (0.8 mol/L), in 70 DEG C of perseverances
3 h are reacted under the conditions of tepidarium, are centrifuged after the reaction was complete, adjusting pH to alkalinity, at 70 DEG C, ultrasound 40 min of heating,
5 ml H are added in every 20 min2O2, after the completion of reaction, centrifuge washing to pH is neutrality, and 10 min of ultrasound are floated
White eucalyptus wood pulp nano-cellulose.As shown in Figure 1, a diameter of 10 ~ 30nm for the nano-cellulose being prepared, length for 100nm ~
10μm。
The effect that NaOH solution used impregnates in the present invention is by lignin and half fiber remaining in bleached eucalyptus pulp
Dimension element removing, the effect of ultrasonic wave added are that the cohesive force of microfibril in fiber is reduced by the physical action that ultrasonic cavitation is steeped, will
Fibrous inside becomes loose, can preferably permeate, and condition is provided for further hydrolysis.
Embodiment 2
6 g bleached eucalyptus pulps are weighed, 5 min is impregnated for 20% NaOH solution with mass fraction, takes out, blended diafiltration
It is 6 ~ 8 to wash to pH, obtains slurry.It is uniformly mixed with 300 ml ammonium persulfate solutions (1.0mol/L), in 80 °C of perseverances
2 h are reacted under the conditions of tepidarium, are centrifuged after the reaction was complete, pH is adjusted to alkalinity, at 70 DEG C, adds in 5 ml H2O2, surpass
20 min of acoustic heating, after the completion of reaction, centrifugation adjusts pH to neutrality, and 10 min of ultrasound obtain bleached eucalyptus pulp Nanowire
Dimension element.Prepared bleached eucalyptus pulp nano-cellulose is freeze-dried, fraction solids is taken out and is ground into powder, is taken few
Powdered samples and KBr co-ground tablettings are measured, carries out FTIR tests, test result is as shown in Figure 2.In addition, after taking drying
5 ~ 10 mg of solid carry out thermogravimetic analysis (TGA) TGA tests in a nitrogen atmosphere, test result is as shown in Figure 3.
A length of 3700~3000 cm of Fig. 2 medium waves-1Between the broad peak that occurs absorbed for the stretching vibration of alcoholic extract hydroxyl group (O-H)
Peak, 2892cm-1 And 1368cm-1The symmetrical and asymmetric stretching vibration peak of respectively C-H, 1605cm-1For the micro- of absorption
Measure the bending vibration of water O-H, 1113 cm-1Locate as stretching vibration in symmetrical phase ring, 1047cm-1 Locate as the flexible of C-O and
Deformation vibration, 621cm-1 Locate the stretching vibration peak that small absorption peak is C-C.These main characteristic absorption peaks show sample
It is cellulose.
From Fig. 3 it is found that being nearby heated at 100 °C for nano-cellulose loses the process of Free water, at 250-450 °
The cracking process of larger weightlessness, predominantly nano-cellulose in this section of C.Prepared bleached eucalyptus pulp nano-cellulose is most
Big weight loss rate point temperature：348.9 °C, residual volume is：29.15%.
Embodiment 3
6 g bleached eucalyptus pulps are weighed, 5 min is impregnated for 10 % NaOH solution with mass fraction, takes out, blended diafiltration
It is 6 ~ 8 to wash to pH, obtains slurry.It is uniformly mixed with 300 ml ammonium persulfate solutions (0.8 mol/L), in 80 DEG C of perseverances
2.5 h are reacted under the conditions of tepidarium, are centrifuged after the reaction was complete, adjust pH to alkalinity, at 70 DEG C, Ultrasonic Heating 40
Min adds in 5ml H every 20 min2O2, after the completion of reaction, centrifugation washing process to pH is neutrality, and 15 min of ultrasound are obtained
To bleached eucalyptus pulp nano-cellulose.
Embodiment 4
6 g bleached eucalyptus pulps are weighed, a night is impregnated for 10 % NaOH solution with mass fraction, takes out, blend filtration washing
To pH slurry is obtained for 6 ~ 8.It is uniformly mixed with 300 ml ammonium persulfate solutions (1.0 mol/L), in 70 DEG C of thermostatted waters
3 h are reacted under the conditions of bath, are centrifuged after the reaction was complete, adjust pH to alkalinity, under 70 °C, 20 min of Ultrasonic Heating is added in
5 ml H2O2, after the completion of reaction, centrifugation washing process to pH is neutrality, and 20 min of ultrasound obtain bleached eucalyptus pulp Nanowire
Dimension element.
Embodiment 5
6 g bleached eucalyptus pulps are weighed, a night is impregnated with tap water, takes out, blend and slurry is obtained by filtration.With 300 ml over cures
Acid ammonium solution (1.0 mol/L) is uniformly mixed, and 3 h are reacted under the conditions of 70 DEG C of waters bath with thermostatic control, is centrifuged, is adjusted after the reaction was complete
PH is saved to alkalinity, under the conditions of 60 DEG C, 60 min of Ultrasonic Heating adds in 5 ml H every 20 min2O2, reaction completion
Afterwards, it centrifuges, adjusts pH to neutrality, 20 min of ultrasound obtain bleached eucalyptus pulp nano-cellulose.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all the present invention
All any modification, equivalent and improvement made within spirit and principle etc., should be included in the protection of the claims in the present invention
Within the scope of.
Claims (8)
1. a kind of preparation method of bleached eucalyptus pulp nano-cellulose, which is characterized in that include the following steps：
(1) bleached eucalyptus pulp in NaOH solution of the mass fraction for 10% ~ 25% is impregnated, obtains prepreg；
(2) prepreg is fully blended, filtration washing obtains slurry；
(3) slurry is uniformly mixed with ammonium persulfate solution, heating stirring is reacted under the conditions of 70 ~ 80 DEG C；
(4) centrifuge washing adds water, adjusts pH to alkalinity；
(5) H is added under the conditions of 60 ~ 70 DEG C2O220 ~ 40 min are stirred by ultrasonic in solution；
(6) centrifuge washing is 6 ~ 8 to pH, and 5 ~ 10 min of ultrasound obtain bleached eucalyptus pulp nano-cellulose suspension.
2. the preparation method of bleached eucalyptus pulp nano-cellulose according to claim 1, which is characterized in that step (1)
In, the soaking time of the bleached eucalyptus pulp is 5 ~ 10 min.
3. the preparation method of bleached eucalyptus pulp nano-cellulose according to claim 1, which is characterized in that step (2)
In, the obtained pH of slurry that washs is 6 ~ 8.
4. the preparation method of bleached eucalyptus pulp nano-cellulose according to claim 1, which is characterized in that step (3)
In, a concentration of 0.8 ~ 1 mol/L of the ammonium persulfate solution, the mass ratio of ammonium persulfate and bleached eucalyptus pulp is 10:1~
2。
5. the preparation method of bleached eucalyptus pulp nano-cellulose according to claim 1, which is characterized in that step (3)
In, the heating reaction time is 2 ~ 3 h.
6. the preparation method of bleached eucalyptus pulp nano-cellulose according to claim 1, which is characterized in that step (4)
In, the pH is 11 ~ 13.
7. the preparation method of bleached eucalyptus pulp nano-cellulose according to claim 1, which is characterized in that step (5)
In, the H2O2 The mass fraction of solution is 20% ~ 30%, the H2O2 The additive amount of solution meets：Step（4）Middle addition water
Volume and H2O2The volume ratio of solution is 40 ~ 50:1.
8. the nano-cellulose based on bleached eucalyptus pulp is prepared by claim 1-7 any one of them preparation methods
Suspension.
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| CN110317370A (en) * | 2019-07-08 | 2019-10-11 | 华南理工大学 | A kind of cationic surfactant modified nanometer cellulose/native rubber composite material and preparation method thereof |
| CN111979817A (en) * | 2020-07-20 | 2020-11-24 | 云南云景林纸股份有限公司 | Method for removing lignin from plant fiber |
| WO2021237382A1 (en) * | 2020-05-23 | 2021-12-02 | 海门茂发美术图案设计有限公司 | Method for preparing bamboo pulp nanocellulose |
| CN115637601A (en) * | 2022-10-10 | 2023-01-24 | 浙江理工大学 | Method for green extraction of high-purity cellulose nanofibers from shaddock peels |
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| CN115637601A (en) * | 2022-10-10 | 2023-01-24 | 浙江理工大学 | Method for green extraction of high-purity cellulose nanofibers from shaddock peels |
| CN115637601B (en) * | 2022-10-10 | 2023-09-29 | 浙江理工大学 | Method for green extraction of high-purity cellulose nanofiber from shaddock ped |
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