CN109762187A - The preparation method of chiral nematic Cellulose nanocrystal body thin film, application - Google Patents
The preparation method of chiral nematic Cellulose nanocrystal body thin film, application Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of chiral nematic Cellulose nanocrystal body thin film, comprising the following steps: (1) the Cellulose nanocrystal body of narrow size distribution and deionized water is taken to be configured to Cellulose nanocrystal liquid solution；(2) the Cellulose nanocrystal liquid solution being prepared in step (1) is ultrasonically treated；(3) the Cellulose nanocrystal liquid solution evaporation self assembly after ultrasonic treatment is formed a film to get chiral nematic Cellulose nanocrystal body thin film is arrived.The present invention correspondingly provides a kind of above-mentioned chiral nematic Cellulose nanocrystal body thin film in the application in intelligent anti-counterfeiting field.The present invention is configured to Cellulose nanocrystal liquid solution using the Cellulose nanocrystal body and deionized water of narrow size distribution, using ultrasonic treatment, evaporation self assembly film forming, a kind of chiral nematic Cellulose nanocrystal body thin film is prepared, which can prepare chiral nematic Cellulose nanocrystal body thin film with controllable precise.
Description
Technical field
The invention belongs to field of polymer composite material more particularly to a kind of preparation sides of Cellulose nanocrystal body thin film
Method, application.
Background technique
For the rod-like fibre element nanocrystal obtained with sulphuric acid hydrolysis because partial size is small, draw ratio has greatly rigidity, surface band
There is the suspension that the reasons such as negative electrical charge (sulfate group) can be stable in water, when the concentration of Cellulose nanocrystal liquid suspension reaches
Ordered arrangement can be self-assembly of by chirality when on to a critical concentration, this ordered arrangement is referred to as chiral nematic
Structure.Also, with the evaporation of solvent, concentration is increased, until moisture evaporating completely forms film, is still able to maintain its chirality
Nematic structure.
Find that the micro-nano structure of cellulose forms chirality in early-stage study nano cellulose crystal self assembling process
Key, the nano cellulose crystal with high length-diameter ratio, rigidity easily form the nano-fiber film with chiral arrangement.In addition,
Self assembly is also a controllable reaction process, and the further investigation for how adjusting nano cellulose crystal self assembly is not carried out also.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, one kind is provided
The preparation method of chiral nematic Cellulose nanocrystal body thin film, the film are organized certainly by Cellulose nanocrystal body, the preparation
Method can realize Cellulose nanocrystal body controllable precise self assembly.In addition, the present invention correspondingly provides a kind of above-mentioned film
Using.In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
A kind of preparation method of chiral nematic Cellulose nanocrystal body thin film, comprising the following steps:
(1) the Cellulose nanocrystal body and deionized water for taking narrow size distribution are configured to Cellulose nanocrystal liquid solution；
(2) the Cellulose nanocrystal liquid solution being prepared in step (1) is ultrasonically treated；
(3) the Cellulose nanocrystal liquid solution evaporation self assembly after ultrasonic treatment is formed a film to get chiral nematic fiber is arrived
Plain nanocrystalline thin film.
In above-mentioned preparation method, it is preferred that the Cellulose nanocrystal body of narrow size distribution refers to that Cellulose nanocrystal body is in
Ellipsoid, and its long axis is 55-200nm, short axle 20-70nm.
In above-mentioned preparation method, it is preferred that the preparation method of the Cellulose nanocrystal body of the narrow size distribution include with
Lower step:
S1: nanofiber micro-crystal powder is obtained into Cellulose nanocrystal liquid suspension by sulphuric acid hydrolysis；
S2: using microjet high pressure homogenization method to the size of Cellulose nanocrystal liquid suspension obtained in step (1) into
Row homogenize process；
S3: anti-dialysis concentration obtains the Cellulose nanocrystal body of narrow size distribution.
In above-mentioned preparation method, it is preferred that sulphuric acid hydrolysis obtains Cellulose nanocrystal liquid suspension the following steps are included: will
Nano-cellulose micro-crystal powder is added in the concentrated sulfuric acid, heating stirring hydrolysis, wait hydrolyze after ultrapure water is added to terminate hydrolysis anti-
It answers, obtains sulfuric acid-treated cellulose mixed solution, cellulose mixed solution is then subjected to high speed centrifugation processing, is removed residual
Remaining acid.
In above-mentioned preparation method, it is preferred that the sulfuric acid concentration is 50-60wt.%；When heating stirring hydrolyzes, control adds
Hot temperature is 40-70 DEG C, mixing speed 200-350r/min, hydrolysis time 0.3-1h；High speed centrifugation processing when, control from
Heart speed is 9000-10000r/min, centrifugation time 5-10min.
In above-mentioned preparation method, it is preferred that when the processing of microjet high pressure homogenization method, pressure 1000-10000MPa, number
It is 5-10 times；Anti- dialysis concentration is the following steps are included: being placed in molecular weight for the Cellulose nanocrystal body after homogenize process and being
It is counter in the polyglycol solution of 20000-100000 to be dialysed, Cellulose nanocrystal bulk concentration is concentrated into 3.5-50wt.%.
The above-mentioned cellulose nanometer that size uniformity, narrow size distribution are prepared for using sulphuric acid hydrolysis joint high pressure homogenization method
Crystal can solve conventional fibre element nanocrystal due to size unevenness by the control of above-mentioned processing step and process conditions
One, the problem of causing difficulty to be self-assembly of chiral nematic structure, not in above-mentioned process conditions, Cellulose nanocrystal body is difficult to meet
This requirement of size uniformity, narrow size distribution.
In above-mentioned preparation method, it is preferred that in the step (1), when Cellulose nanocrystal body is configured to solution, control is gone
The mass ratio of ionized water and Cellulose nanocrystal body is (20-200): 1, and agitating solution 5-10min.Studies have shown that above-mentioned go
The control of ionized water and the mass ratio of Cellulose nanocrystal body is extremely important, and Cellulose nanocrystal liquid solution concentration affects fiber
The viscosity of plain nanocrystal solution changes the mobility of Cellulose nanocrystal body by adjusting concentration, can control self assembly, fine
The concentration for tieing up plain nanocrystal solution is to realize an essential condition of self assembly, above or below all can not achieve self assembly.
The effect of stirring is that the Cellulose nanocrystal weight that makes to reunite originally is newly fully dispersed in the solution, and the time not enough will lead to dispersion
Not exclusively.
In above-mentioned preparation method, it is preferred that in the step (2), when ultrasonic treatment, control ultrasonic power is 400-
1600W, ultrasonic time 5-20min.There may be complete without dialysis after sulphuric acid hydrolysis around Cellulose nanocrystal body
Plasma, the presence of these ions will squeeze static layer, and the electrostatic repulsion between shielding fiber element nanocrystal.Ultrasonic treatment
It is to transmit energy to Cellulose nanocrystal body, breaks up ion, makes the electrostatic between Cellulose nanocrystal body that layer be denounceed to reduce, to reduce
Torsion angle between Cellulose nanocrystal body layer, to carry out self assembly regulation, ultrasonic power cannot be excessively high, excessively high energy
It is excessively high that input will lead to local temperature, so as to cause Cellulose nanocrystal body desulfurization perester radical, hinders self assembly.
In above-mentioned preparation method, it is preferred that in the step (3), when evaporation, control evaporating temperature is 20-45 DEG C.Evaporation
Temperature condition in Cellulose nanocrystal body self assembling process thermodynamic behavior and dynamic behavior have important influence, steam
Send out that temperature is too low, solution evaporation it is relatively slow, it is difficult to be self-assembly of chiral nematic structure, evaporating temperature is excessively high, solvent volatilization
Too fast, cellulose has little time to be self-assembly of chiral nematic structure.
As a general technical idea, the present invention also provides a kind of chiral nematic celluloses that above-mentioned preparation method obtains
Application of the nanocrystalline thin film in intelligent anti-counterfeiting field.
We are studies have shown that the formation of chiral nematic Cellulose nanocrystal body thin film is a complicated thermodynamics and power
The process of balance is learned, it is related with type, rate of volatilization, the ultrasonic treatment condition of solvent etc..Method in through the invention, can be with
The controllableization self assembly for realizing Cellulose nanocrystal body obtains a kind of chiral nematic cellulose that can be used for intelligent anti-counterfeiting field and receives
Rice crystal film.
Compared with the prior art, the advantages of the present invention are as follows:
1, the present invention is configured to Cellulose nanocrystal body using the Cellulose nanocrystal body and deionized water of narrow size distribution
A kind of chiral nematic Cellulose nanocrystal body thin film has been prepared using ultrasonic treatment, evaporation self assembly film forming in solution,
The preparation method can prepare chiral nematic Cellulose nanocrystal body thin film with controllable precise.
2, preparation method of the invention is simple, at low cost, and without toxic organic reagent as solvent, to environment
It is all safe from harm with production operation personnel.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the polarisation test chart of the Cellulose nanocrystal body thin film obtained under various concentration in embodiment 1.
Fig. 2 is the polarisation test chart of the Cellulose nanocrystal body thin film obtained under different ultrasound conditions in embodiment 2.
Fig. 3 is the polarisation test chart of the Cellulose nanocrystal body thin film obtained under different evaporating temperatures in embodiment 3.
Fig. 4 is the polarisation test chart of Cellulose nanocrystal body thin film obtained in comparative example 1.
Fig. 5 is the polarisation test chart of Cellulose nanocrystal body thin film obtained in embodiment 4.
Specific embodiment
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
A kind of preparation method of chiral nematic Cellulose nanocrystal body thin film, comprising the following steps:
(1) the Cellulose nanocrystal body 10g of the size uniformity, narrow size distribution that weigh five parts of 5.9wt.% is in beaker, so
Deionized water is added afterwards respectively by its concentration dilution to 4.5wt.%, 3.5wt.%, 2.5wt.%, 1.5wt.%, 0.5wt.%；
(2) 8min is stirred with glass bar respectively, is uniformly mixed it；
(3) the Cellulose nanocrystal body of various concentration is subjected to ice-water bath ultrasound, ultrasonic power 540W, ultrasonic time respectively
5min；
(4) ultrasound finishes, and respectively retains 5g Cellulose nanocrystal liquid suspension after sample is cooling, places at room temperature
Slow drying and forming-film.
Size uniformity in the present embodiment, narrow size distribution Cellulose nanocrystal body the preparation method is as follows:
(1) it weighs 2.50g nanofiber micro-crystal powder to be added in three-necked flask, and the concentrated sulfuric acid of 50wt.% is added
100mL reacts 0.4h with the stirring of 250r/min revolving speed at 40 DEG C；The burning equipped with 1000mL deionized water is poured into after having hydrolyzed
In cup, stops sulphuric acid hydrolysis, obtain white " milky " liquid；Then obtained white " milky " liquid is subjected to centrifugal treating, removes big portion
Divide remaining sulfuric acid, is centrifuged 10min at 9000r/min, removes supernatant, lower sediment deionized water is dispersed again, obtained
To Cellulose nanocrystal liquid suspension；
(2) Cellulose nanocrystal liquid suspension is poured into microjet high pressure homogenizer under 5000MPa pressure, processing 10
It is secondary, obtain the Cellulose nanocrystal liquid solution of size uniformity；
(3) taking molecular weight is that 20000 Liquid Macrogol g is added in 1L deionized water, under the conditions of 45 DEG C, stirring
It makes it completely dissolved, obtains anti-dialyzate；Then the Cellulose nanocrystal liquid solution after homogenization is packed into molecular weight is
It in 1000 bag filter, is immersed in anti-dialyzate completely 3 days, takes out bag filter to get to size uniformity, narrow size distribution
Cellulose nanocrystal liquid solution (concentration of control Cellulose nanocrystal body is 5.9wt.%).
Embodiment 2:
A kind of preparation method of chiral nematic Cellulose nanocrystal body thin film, comprising the following steps:
(1) weigh the size uniformity of 5.9wt.%, narrow size distribution Cellulose nanocrystal body 80g in beaker, then plus
Enter deionized water for its concentration dilution to 2.5wt.%；
(2) 10min is stirred with glass bar respectively, is uniformly mixed it；
(3) the Cellulose nanocrystal liquid solution after taking eight parts of stirrings, every part of 10g；
(4) ultrasonic under the conditions of ice-water bath, wherein four parts of ultrasonic time 5min, ultrasonic power be respectively 400W, 800W,
1200W,1600W；Other four parts of ultrasonic power is 600W, ultrasonic time 5min, 10min, 15min, 20min；
(5) ultrasound finishes, and respectively retains 5g Cellulose nanocrystal liquid suspension after sample is cooling, places at room temperature
Slow drying and forming-film.
Size uniformity in the present embodiment, narrow size distribution Cellulose nanocrystal body the preparation method is the same as that of Example 1.
Embodiment 3:
A kind of preparation method of chiral nematic Cellulose nanocrystal body thin film, comprising the following steps:
(1) weigh the size uniformity of 5.9wt.%, narrow size distribution Cellulose nanocrystal body 30g in beaker, then plus
Enter deionized water for its concentration dilution to 2.5wt.%；
(2) 5min is stirred with glass bar respectively, is uniformly mixed it；
(3) the Cellulose nanocrystal liquid solution after taking three parts of stirrings, every part of 10g；
(4) ultrasonic under the conditions of ice-water bath, ultrasonic time 5min, ultrasonic power 540W；
(5) ultrasound finishes, and respectively retains 5g Cellulose nanocrystal liquid suspension after sample is cooling, be individually positioned in 35 DEG C,
Slow drying and forming-film under the conditions of 40 DEG C and 45 DEG C.
Size uniformity in the present embodiment, narrow size distribution Cellulose nanocrystal body the preparation method is the same as that of Example 1.
Embodiment 4:
A kind of preparation method of chiral nematic Cellulose nanocrystal body thin film, comprising the following steps:
(1) weigh the size uniformity of 5.9wt.%, narrow size distribution Cellulose nanocrystal body 30g in beaker, then plus
Enter deionized water for its concentration dilution to 3.0wt.%；
(2) 5min is stirred with glass bar respectively, is uniformly mixed it；
(3) the Cellulose nanocrystal liquid solution after taking three parts of stirrings, every part of 10g；
(4) ultrasonic under the conditions of ice-water bath, ultrasonic time 10min, ultrasonic power 700W；
(5) ultrasound finishes, and respectively retains 5g Cellulose nanocrystal liquid suspension after sample is cooling, is individually positioned in 30 DEG C of items
Slow drying and forming-film under part.
Size uniformity in the present embodiment, narrow size distribution Cellulose nanocrystal body the preparation method is the same as that of Example 1.
Comparative example 1:
A kind of preparation method of Cellulose nanocrystal body thin film, comprising the following steps:
(1) weigh the size uniformity of 5.9wt.%, narrow size distribution Cellulose nanocrystal body 30g in beaker, then plus
Enter deionized water for its concentration dilution to 2.5wt.%；
(2) 5min is stirred with glass bar respectively, is uniformly mixed it；
(3) the Cellulose nanocrystal liquid solution 5g after taking stirring, slow drying and forming-film under the conditions of being placed on 80 DEG C.
Size uniformity in this comparative example, narrow size distribution Cellulose nanocrystal body the preparation method is the same as that of Example 1.
Using petrographic microscope to the obtained chiral nematic Cellulose nanocrystal in above-described embodiment 1-3 and comparative example 1
The polarisation property of body thin film is tested, as shown in Figs 1-4 respectively.Cellulose nanocrystal body waving with solvent as shown in Figure 1
Hair, the chiral nematic structure of Cellulose nanocrystal body are retained, and also there is no large changes for polarizing properties, therefore can
To change the polarity of the dry rear film of Cellulose nanocrystal soma by concentration.As shown in Figure 2 in ultrasonic power 600W, ultrasound
Petrographic microscope is mainly observed green when 5min, with the increase of ultrasonic time, by polarized light microscope observing to gradually becoming
Red, as ultrasonic 15min, what is seen with petrographic microscope is essentially all red.In ultrasonic time 5min, ultrasonic power 400W
When, polarized light microscopy photo is concentrated mainly on blue.With the increase of ultrasonic power, color by blue gradually change to green, yellow,
Red is arrived again, and the rule regulated and controled with ultrasonic time to it is consistent.Ultrasound leads to polarizing properties red shift, this may be because of cellulose
There may be, without complete plasma of dialysing, the presence of these ions will squeeze quiet after sulphuric acid hydrolysis around nanocrystal
State layer, and the electrostatic repulsion between shielding fiber element nanocrystal.Chirality is formed by under different dry temperature strip parts as shown in Figure 3
There are biggish differences for nematic Cellulose nanocrystal body thin film polarisation photo.As the temperature rises, there is the trend of red shift.
This may be because as the temperature rises, maximum system energy rises, and solvent rate of volatilization is accelerated, so that accelerating fibers element is nanocrystalline
The chiral self assembling process of body, screw pitch increase, and corresponding change has occurred in polarizing properties.Cellulose nanometer is obtained as shown in Figure 4
Crystal film is not self-assembly of chiral nematic structure without polarity.
Cellulose nanocrystal body thin film obtained in embodiment 4 can show specific at specific position under petrographic microscope
Color as shown in figure 5, carrying out corresponding digital coding, Bian Keyong for Cellulose nanocrystal body thin film obtained in embodiment 4
Make information storage or antifalsification label.
Comparative example 2:
A kind of preparation method of Cellulose nanocrystal body thin film, comprising the following steps:
(1) weigh the size uniformity of 5.9wt.%, narrow size distribution Cellulose nanocrystal body 10g in beaker, then plus
Enter deionized water for its concentration dilution to 0.3wt.%；
(2) 5min is stirred with glass bar, is uniformly mixed it；
(3) the Cellulose nanocrystal liquid solution after taking three parts of stirrings, every part of 10g；
(4) ultrasonic under the conditions of ice-water bath, ultrasonic time 10min, ultrasonic power 700W；
(5) ultrasound finishes, and respectively retains 5g Cellulose nanocrystal liquid suspension after sample is cooling, is individually positioned in 30 DEG C of items
Slow drying and forming-film under part.
Size uniformity in this comparative example, narrow size distribution Cellulose nanocrystal body the preparation method is the same as that of Example 1.
Cellulose nanocrystal body thin film obtained in this comparative example is not self-assembly of chiral nematic knot without polarity
Structure.
Claims (10)
1. a kind of preparation method of chiral nematic Cellulose nanocrystal body thin film, which comprises the following steps:
(1) the Cellulose nanocrystal body and deionized water for taking narrow size distribution are configured to Cellulose nanocrystal liquid solution；
(2) the Cellulose nanocrystal liquid solution being prepared in step (1) is ultrasonically treated；
(3) the Cellulose nanocrystal liquid solution evaporation self assembly after ultrasonic treatment is formed a film and is received to get to chiral nematic cellulose
Rice crystal film.
2. preparation method according to claim 1, which is characterized in that the Cellulose nanocrystal body of narrow size distribution refers to fibre
Tieing up plain nanocrystal is in ellipsoid, and its long axis is 55-200nm, short axle 20-70nm.
3. preparation method according to claim 1, which is characterized in that the Cellulose nanocrystal body of the narrow size distribution
Preparation method the following steps are included:
S1: nanofiber micro-crystal powder is obtained into Cellulose nanocrystal liquid suspension by sulphuric acid hydrolysis；
S2: it is carried out using size of the microjet high pressure homogenization method to Cellulose nanocrystal liquid suspension obtained in step (1) equal
Matterization processing；
S3: anti-dialysis concentration obtains the Cellulose nanocrystal body of narrow size distribution.
4. preparation method according to claim 3, which is characterized in that sulphuric acid hydrolysis obtains Cellulose nanocrystal liquid suspension
The following steps are included: nano-cellulose micro-crystal powder is added in the concentrated sulfuric acid, heating stirring hydrolysis, wait hydrolyze after be added it is super
Pure water terminates hydrolysis, obtains sulfuric acid-treated cellulose mixed solution, and cellulose mixed solution is then carried out high speed
Centrifugal treating removes remaining acid.
5. the preparation method according to claim 4, which is characterized in that the sulfuric acid concentration is 50-60wt.%；Heating is stirred
When mixing hydrolysis, control heating temperature is 40-70 DEG C, mixing speed 200-350r/min, hydrolysis time 0.3-1h；High speed from
When heart processing, control centrifugal speed is 9000-10000r/min, centrifugation time 5-10min.
6. preparation method according to claim 3, which is characterized in that when the processing of microjet high pressure homogenization method, pressure is
1000-10000MPa, number are 5-10 times；Anti- dialysis concentration is the following steps are included: by the cellulose nanometer after homogenize process
Crystal is placed in molecular weight and is dialysed to be counter in the polyglycol solution of 20000-100000, and Cellulose nanocrystal bulk concentration is dense
It is reduced to 3.5-50wt.%.
7. preparation method according to claim 1 to 6, which is characterized in that in the step (1), cellulose is received
When meter Jing Ti is configured to solution, the mass ratio of control deionized water and Cellulose nanocrystal body is (20-200): 1, and stir molten
Liquid 5-10min.
8. preparation method according to claim 1 to 6, which is characterized in that in the step (2), ultrasonic treatment
When, control ultrasonic power is 400-1600W, ultrasonic time 5-20min.
9. preparation method according to claim 1 to 6, which is characterized in that in the step (3), when evaporation,
Controlling evaporating temperature is 20-45 DEG C.
10. a kind of chiral nematic Cellulose nanocrystal body that preparation method as claimed in any one of claims 1-9 wherein obtains is thin
Application of the film in intelligent anti-counterfeiting field.
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| CN113045787A (en) * | 2021-04-07 | 2021-06-29 | 陕西科技大学 | Preparation method of nano cellulose liquid crystal paper with optical limiting characteristic |
| CN114316373A (en) * | 2021-12-20 | 2022-04-12 | 中国农业大学 | Preparation method of humidity-responsive nano-cellulose composite film and obtained product |
| CN115477777A (en) * | 2022-10-11 | 2022-12-16 | 烟台南山学院 | Preparation method of cellulose nanocrystal film |
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Application publication date: 20190517 |