CN106084135A - Humidity based on Cellulose nanocrystal response photon crystal material and preparation method thereof - Google Patents
Humidity based on Cellulose nanocrystal response photon crystal material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of humidity based on Cellulose nanocrystal response photon crystal material and preparation method thereof, belong to material science.Present invention Cellulose nanocrystal suspension based on cholesteric liquid crystal, by mixing with polybenzazole precursor liquid solution, heat polymer polymerizing, and by the chemical bond interconnection function of cross-linking agent, making polymer and Cellulose nanocrystal keep stable connection and retain the special classification photon structure of itself, the film composite material obtained after solvent volatile dry has obvious humidity response color shifting properties.Compared with prior art, Responsive photonic crystals material prepared by the present invention has special hierarchy, has good response characteristic at humidity responder's mask, has potential application prospect in terms of chemical sensitisation field.
Description
Technical field
The invention belongs to materials science field, especially relate to a kind of humidity response light based on Cellulose nanocrystal
Sub-crystalline material and preparation method thereof.
Background technology
Cellulose nanocrystal is a kind of by the nano material suspension obtained by cellulose acidolysis, cellulose be a kind of by
D-Glucose connects the linear macromolecule polysaccharide of composition with β-Isosorbide-5-Nitrae-glycosidic bond, has crystallization inside natural cellulosic materials simultaneously
District and amorphous area, glucose ring adjacent in crystal region is mutually inverted, rich in hydroxyl, the most adjacent molecule interchain in sugar ring
Or intramolecule is easily formed hydrogen bond, its Stability Analysis of Structures.And amorphous area can pass through strong acid acidolysis, therefore by this processing procedure energy
Access the cellulose crystalline region of needle-like, i.e. Cellulose nanocrystal, its length between 100-300nm, a diameter of 5-15nm.In acid
The part of hydroxyl of solution preocess Middle molecule chain side chain can be with acid reaction, and therefore obtained Cellulose nanocrystal surface is with strong negative
Electricity, therefore, it is possible to stable suspersion is in water.When its concentration reaches to a certain degree, due to the nanocrystalline mutual row of band identical charges
Scolding, its suspension can be self-assembly of the liquid crystal structure of cholesteric phase.This structure has One Dimension Periodic arrangement rule, therefore exists
Under ambient light is shone, its half pitch meets Bragg diffraction formula, regulates and controls its pitch and its diffraction maximum can be made to fall in visible region
In, and then form photonic crystal effect.
It is extensive that Cellulose nanocrystal has raw material sources, nontoxic good characteristic, and the cholesteric phase liquid itself formed
Crystalline substance has special birefringent phenomenon, it is possible to polarized light is produced selection effect, is a kind of excellent photon structure, it is possible to application
In photon sensory field.Special cholesteric liquid crystal structure based on Cellulose nanocrystal, when introducing other multiple response functions
After material, due to the coupling effect of structure Yu performance, or the special nature of cellulose itself, it is possible to prepare have multiple special
The photon crystal material of performance.As at Mark J.MacLachlan in 2013 et al. at " Angew.Chem.Int.Ed. " the 52nd
Response photon gel based on Cellulose nanocrystal is reported by the phase page 8912.Different types of response is polymerized
Thing is combined with Cellulose nanocrystal, obtains the photon gel rubber material with cholesteric liquid crystal structure after solvent is evaporated,
This material can produce swelling/shrinkage phenomenon after changing external condition, causes its pitch to change, therefore, it is possible to as multiple
The sensor of stimulus signal.Such as after being combined with Cellulose nanocrystal by polyacrylamide, it is at aqueous solvent and at spirit solvent
In can produce great colour contrast, this color is controlled by the proportion of composing of mixed solvent, and this is due to polyacrylamide easily
Water absorption and swelling, and poor to alcohol absorption, therefore, it is possible to water and the ethanol of different content in solvent are done and detects targetedly.
Be similar to, Mark P.Andrews etc. at " Sensors and Actuators B:Chemical " in 2013
176 phases page 692 response performance to Cellulose nanocrystal thin film has been also carried out relevant report.Research finds, due to fiber
Element is nanocrystalline itself also has certain absorption characteristic to steam, and therefore itself just can be as the response to air humidity
Sensor.
But, so far, the humidity Responsive photonic crystals prepared based on Cellulose nanocrystal still suffers from deficiency, one
It is that Cellulose nanocrystal is owing to water-soluble excellence, therefore excessive when ambient humidity or that cellulose is nanocrystalline material is straight
During contact water, itself is the most swelling dissolves the most again, causes sensor properties unstable；It two is so far
Its response performance of the report in terms of humidity response still suffer from deficiency, response is poor, seriously limits its actual application.For solving
Certainly above-mentioned deficiency, the present invention is combined with responsive polymer by Cellulose nanocrystal, and is transferred by the chemical bond of cross-linking agent
Connect effect, solve the problems referred to above.
Summary of the invention
The purpose of the present invention, the first overcomes humidity based on Cellulose nanocrystal response photon crystal stability deficiency
Shortcoming, it two is an up its problem as humidity response sensor poor-performing.The present invention utilizes the bonding effect of cross-linking agent,
Polymer is grafted in the way of chemical bonds Cellulose nanocrystal surface, is greatly improved its stability, simultaneously because
Introduce water absorption properties more preferably polymer so that it is under humidity changes, its volume sweell(ing)/shrinkage degree is greatly increased,
Strengthen its response characteristic to humidity.
The purpose of the present invention can be achieved through the following technical solutions:
The preparation method of a kind of humidity based on Cellulose nanocrystal response photon crystal material, to have cholesteric liquid crystal
The Cellulose nanocrystal of characteristic is template, by the chemical bond interconnection function of cross-linking agent, forms chemistry with high polymer monomer and is bonded
Connect, make high polymer monomer be polymerized by heating, and after transpiring moisture, obtain the composite material film with shining color, this thin film
There is humidity response color shifting properties and keep the cholesteric liquid crystal structure of Cellulose nanocrystal.
Preparation method specifically includes following steps:
(1) preparation of Cellulose nanocrystal suspension: cellulose is soaked in acid heating and carries out acidolysis, after acidolysis completes
Dilute terminates acidolysis, takes lower sediment after standing, makes pH stable with dialysis after clean water, obtains cellulose suspension
Liquid；
(2) prepared polymer precursor solution: described polybenzazole precursor liquid solution comprises high polymer monomer, cross-linking agent and draws
Send out agent, and the mass ratio of high polymer monomer, cross-linking agent and initiator be 1:(0.01-0.02): (0.01-0.03), preparation polymerization
Thing precursor solution solvent for use is water, and high polymer monomer concentration in polybenzazole precursor liquid solution is 0.1-0.8mol/L；
(3) take a certain amount of Cellulose nanocrystal suspension, mix with above-mentioned polybenzazole precursor liquid solution, by controlling two
Person's ratio controls the content of polymer, is subsequently heated and carries out polyreaction；
(4) mixing suspension after step (3) being processed is transferred in culture dish, makes moisture evaporation dry in the air under field conditions (factors)
Dry, finally give the composite material film with gorgeous color, this thin film has humidity response color shifting properties and keeps cellulose
Nanocrystalline cholesteric liquid crystal structure.
Further, described Cellulose nanocrystal is obtained by cellulosic raw material passes through acidolysis.Described cellulose
Selected from Cotton Gossypii, Bacterial cellulose or paper pulp fiber.
Further, carrying out the used acid of acidolysis in step (1) is hydrochloric acid, nitric acid or sulphuric acid, and mass fraction is 50-
70%；When carrying out acidolysis operation in step (1), acidolysis temperature is 50-70 DEG C, and heat time heating time is 0.5-2 hour.
Further, described cross-linking agent is the little molecule that two ends have the functional group of reactivity, is preferably selected from penta 2
Aldehyde, ethylene glycol, Biformyl or 1,3-propanedicarboxylic acid.
Further, described high polymer monomer is the monomer with water absorption character polymer, be preferably selected from acrylic acid, third
Acrylamide or N-isopropylacrylamide.
Further, described initiator is preferably selected from potassium peroxydisulfate, Ammonium persulfate. or azodiisobutyronitrile.
Further, in step (3), Cellulose nanocrystal suspension mixes with polybenzazole precursor liquid solution, and polymerization is anti-
Ying Hou, the mass fraction of polymer is 5-40%, the polymer that described polymer is formed after referring to high polymer monomer polymerization.
Further, carrying out the heating-up temperature needed for polyreaction and be 40-60 DEG C in step (3), heat time heating time is that 2-6 is little
Time.
Compared with prior art, the present invention with there is cholesteric liquid crystal structure Cellulose nanocrystal as template, by hand over
Connection agent bonding effect, with have response polymer be combined, utilize Cellulose nanocrystal itself from group leader's characteristic, be prepared for
There is the humidity Responsive photonic crystals material of cholesteric liquid crystal structure.This material is in response cycle stability and response performance side
Mask has certain advantage.When extraneous relative humidity rises, the water absorption and swelling of polymer own, cause cholesteric liquid crystal structure
Pitch increases, and therefore the reflection peak of its reflectance spectrum there will be obvious Red Shift Phenomena, and vice versa.Utilize Cellulose nanocrystal
The special nature of itself, this preparation method can be applied to the preparation of other multiple Responsive photonic crystals, at erasable photon
The fields such as paper, sensor, false proof, decoration have potential application prospect.
Accompanying drawing explanation
Fig. 1 is polarizing microscope photo based on Cellulose nanocrystal suspension；
Fig. 2 is the stereoscan photograph of humidity based on Cellulose nanocrystal response photon crystal material；
Fig. 3 is the humidity response characteristic of humidity based on Cellulose nanocrystal response photon crystal material, its reflectance spectrum
Having significantly change under different humidity, optical microscope photograph shows that its color is affected by humidity.
Detailed description of the invention
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The first step, the preparation of Cellulose nanocrystal suspension: cellulose is soaked in the concentrated sulfuric acid solution of 60% heating
Hydrolysis, heating-up temperature is 60 DEG C, and heat time heating time is 2 hours, has hydrolyzed rear dilute and has terminated hydrolysis, takes off layer and sink after standing
Forming sediment, with clean water centrifugal 3-4 time, then dialysis makes pH stable, obtains cellulose suspension, through this fibre knowable to test
The concentration of dimension element suspension is 3%；
Second step, prepared polymer precursor solution: take acrylamide monomer 1g, glutaraldehyde (cross-linking agent) 40 μ L, over cure
Acid potassium 0.01g, is dissolved in 28mL water, and the concentration of high polymer monomer controls, at 0.5mol/L, to complete the configuration of precursor solution；
3rd step, takes Cellulose nanocrystal suspension 5mL of preparation in the first step, takes the precursor solution of second step configuration
420 μ L, by both mix homogeneously, understand polymer content by calculating and are about 10%.Afterwards mixed solution is sealed and 60 DEG C
Heating in water bath 4 hours；
4th step, is transferred to the mixing suspension after three step process in culture dish, makes moisture steam under field conditions (factors)
Sending out and dry, finally give the composite material film with gorgeous color, this thin film has humidity response color shifting properties and keeps fine
The cholesteric liquid crystal structure that dimension element is nanocrystalline.
Fig. 1 is polarizing microscope photo based on Cellulose nanocrystal suspension, it appeared that have obvious birefringence
Phenomenon, it was demonstrated that its suspension has liquid crystal structure；
Fig. 2 is the stereoscan photograph of humidity based on Cellulose nanocrystal response photon crystal material, and it is dried
Thin film has the liquid crystal structure of cholesteric phase, and this multi-layer film structure makes it have obvious photonic crystal properties；
Fig. 3 is the humidity response characteristic of humidity based on Cellulose nanocrystal response photon crystal material, by reflectance spectrum
Understanding with optical microscope photograph, its schemochrome is affected by humidity: when humidity rises, and the water absorption and swelling of polymer own causes
The pitch of cholesteric liquid crystal structure increases, and therefore the reflection peak of its reflectance spectrum there will be obvious Red Shift Phenomena, otherwise also
So..
Embodiment 2
The first step, the preparation of Cellulose nanocrystal suspension: cellulose is soaked in the concentrated hydrochloric acid solution of 70% heating
Hydrolysis, heating-up temperature is 50 DEG C, and heat time heating time is 2 hours, has hydrolyzed rear dilute and has terminated hydrolysis, takes off layer and sink after standing
Forming sediment, with clean water centrifugal 3-4 time, then dialysis makes pH stable, obtains cellulose suspension, through this fibre knowable to test
The concentration of dimension element suspension is 3%；
Second step, prepared polymer precursor solution: take acrylamide monomer 1g, glutaraldehyde (cross-linking agent) 40 μ L, over cure
Acid potassium 0.01g, is dissolved in 28mL water, and the concentration of high polymer monomer controls, at 0.5mol/L, to complete the configuration of precursor solution；
3rd step, takes Cellulose nanocrystal suspension 5mL of preparation in the first step, takes the precursor solution of second step configuration
1mL, by both mix homogeneously, understands polymer content by calculating and is about 20%.Afterwards mixed solution is sealed and 65 DEG C of water
Bath heating 2 hours；
4th step, is transferred to the mixing suspension after three step process in culture dish, makes moisture steam under field conditions (factors)
Sending out and dry, finally give the composite material film with gorgeous color, this thin film has humidity response color shifting properties and keeps fine
The cholesteric liquid crystal structure that dimension element is nanocrystalline.
Embodiment 3
The first step, the preparation of Cellulose nanocrystal suspension: cellulose is soaked in the concentrated sulfuric acid solution of 60% heating
Hydrolysis, heating-up temperature is 60 DEG C, and heat time heating time is 2 hours, has hydrolyzed rear dilute and has terminated hydrolysis, takes off layer and sink after standing
Forming sediment, with clean water centrifugal 3-4 time, then dialysis makes pH stable, obtains cellulose suspension, through this fibre knowable to test
The concentration of dimension element suspension is 3%；
Second step, prepared polymer precursor solution: take acrylamide monomer 2g, 1,3-propanedicarboxylic acid (cross-linking agent) 80 μ L, azo
Bis-isobutyronitrile 0.03g, is dissolved in 28mL water, and the concentration of high polymer monomer controls, at 1mol/L, to complete the configuration of precursor solution；
3rd step, takes Cellulose nanocrystal suspension 10mL of preparation in the first step, and the presoma taking second step configuration is molten
Liquid 200 μ L, by both mix homogeneously, understands polymer content by calculating and is about 8%.Afterwards mixed solution is sealed and 60 DEG C
Heating in water bath 4 hours；
4th step, is transferred to the mixing suspension after three step process in culture dish, makes moisture steam under field conditions (factors)
Sending out and dry, finally give the composite material film with gorgeous color, this thin film has humidity response color shifting properties and keeps fine
The cholesteric liquid crystal structure that dimension element is nanocrystalline.
Embodiment 4
The first step, the preparation of Cellulose nanocrystal suspension: cellulose is soaked in the concentrated sulfuric acid solution of 65% heating
Hydrolysis, heating-up temperature is 65 DEG C, and heat time heating time is 1.5 hours, has hydrolyzed rear dilute and has terminated hydrolysis, has taken off layer after standing
Precipitation, with clean water centrifugal 3-4 time, then dialysis makes pH stable, obtains cellulose suspension, knowable to test this
The concentration of cellulose suspension is 3%；
Second step, prepared polymer precursor solution: take N-isopropylacrylamide monomer 0.5g, glutaraldehyde (cross-linking agent) 40
μ L, potassium peroxydisulfate 0.01g, be dissolved in 4mL water, and the concentration of high polymer monomer controls, at 1mol/L, to complete joining of precursor solution
Put；
3rd step, takes Cellulose nanocrystal suspension 5mL of preparation in the first step, takes the precursor solution of second step configuration
0.5mL, by both mix homogeneously, understands polymer content by calculating and is about 30%.Afterwards mixed solution is sealed and 65 DEG C
Heating in water bath 1 hour；
4th step, is transferred to the mixing suspension after three step process in culture dish, makes moisture steam under field conditions (factors)
Sending out and dry, finally give the composite material film with gorgeous color, this thin film has humidity response color shifting properties and keeps fine
The cholesteric liquid crystal structure that dimension element is nanocrystalline.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and use invention.
These embodiments obviously easily can be made various amendment by person skilled in the art, and described herein typically
Principle is applied in other embodiments without through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel should be the present invention's according to the announcement of the present invention, the improvement made without departing from scope and amendment
Within protection domain.
Claims (10)
1. the preparation method of humidity based on a Cellulose nanocrystal response photon crystal material, it is characterised in that to have
The Cellulose nanocrystal of cholesteric liquid crystal characteristic is template, by the chemical bond interconnection function of cross-linking agent, with high polymer monomer shape
Become chemical bond to connect, make high polymer monomer be polymerized by heating, and after transpiring moisture, obtain the composite with shining color
Thin film, this thin film has humidity response color shifting properties and keeps the cholesteric liquid crystal structure of Cellulose nanocrystal.
The preparation side of a kind of humidity based on Cellulose nanocrystal the most according to claim 1 response photon crystal material
Method, it is characterised in that preparation method specifically includes following steps:
(1) preparation of Cellulose nanocrystal suspension: cellulose being soaked in acid heating and carries out acidolysis, acidolysis adds water after completing
Dilution terminates acidolysis, takes lower sediment after standing, and after cleaning, dialysis makes pH stable, obtains cellulose suspension；
(2) prepared polymer precursor solution: described polybenzazole precursor liquid solution comprises high polymer monomer, cross-linking agent and initiation
Agent, and the mass ratio of high polymer monomer, cross-linking agent and initiator is 1:(0.01-0.02): (0.01-0.03), high polymer monomer
Concentration in polybenzazole precursor liquid solution is 0.1-0.8mol/L；
(3) take a certain amount of Cellulose nanocrystal suspension, mix with above-mentioned polybenzazole precursor liquid solution, compare both controlling
Example controls the content of polymer, is subsequently heated and carries out polyreaction；
(4) by step (3) process after mixing suspension, make under field conditions (factors) moisture evaporation dry, finally give have gorgeous
The composite material film of beautiful color, this thin film has humidity response color shifting properties and keeps the cholesteric liquid crystal of Cellulose nanocrystal
Structure.
The preparation side of a kind of humidity based on Cellulose nanocrystal the most according to claim 2 response photon crystal material
Method, it is characterised in that described cellulose is selected from Cotton Gossypii, Bacterial cellulose or paper pulp fiber.
The preparation side of a kind of humidity based on Cellulose nanocrystal the most according to claim 2 response photon crystal material
Method, it is characterised in that carrying out the used acid of acidolysis in step (1) is hydrochloric acid, nitric acid or sulphuric acid, mass fraction is 50-
70%；
When carrying out acidolysis operation in step (1), acidolysis temperature is 50-70 DEG C, and heat time heating time is 0.5-2 hour.
The preparation of a kind of humidity based on Cellulose nanocrystal the most according to claim 1 and 2 response photon crystal material
Method, it is characterised in that described cross-linking agent is the little molecule that two ends have the functional group of reactivity, selected from glutaraldehyde, second
Glycol, Biformyl or 1,3-propanedicarboxylic acid.
The preparation of a kind of humidity based on Cellulose nanocrystal the most according to claim 1 and 2 response photon crystal material
Method, it is characterised in that described high polymer monomer is the monomer with water absorption character polymer, selected from acrylic acid, acryloyl
Amine or N-isopropylacrylamide.
The preparation side of a kind of humidity based on Cellulose nanocrystal the most according to claim 2 response photon crystal material
Method, it is characterised in that described initiator is potassium peroxydisulfate, Ammonium persulfate. or azodiisobutyronitrile.
The preparation side of a kind of humidity based on Cellulose nanocrystal the most according to claim 2 response photon crystal material
Method, it is characterised in that in step (3), Cellulose nanocrystal suspension mixes with polybenzazole precursor liquid solution, and polyreaction
After, the mass fraction of polymer is 5-40%, the polymer that described polymer is formed after referring to high polymer monomer polymerization.
The preparation side of a kind of humidity based on Cellulose nanocrystal the most according to claim 2 response photon crystal material
Method, it is characterised in that carry out the heating-up temperature needed for polyreaction in step (3) and be 40-60 DEG C, heat time heating time is 2-6 hour.
10. the humidity based on Cellulose nanocrystal using preparation method according to any one of claim 1-9 to prepare is rung
Answer photon crystal material.
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| CN110218360A (en) * | 2019-05-31 | 2019-09-10 | 华南理工大学 | A kind of flexible waterproof CNC/PEGDA photon crystal material and preparation method thereof |
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| CN110218360A (en) * | 2019-05-31 | 2019-09-10 | 华南理工大学 | A kind of flexible waterproof CNC/PEGDA photon crystal material and preparation method thereof |
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| CN111040225A (en) * | 2019-12-05 | 2020-04-21 | 中山大学 | Repeatedly erasable anti-counterfeiting film based on photonic crystal structural color and preparation method and application thereof |
| CN112795043A (en) * | 2021-02-01 | 2021-05-14 | 湖州闪思新材料科技有限公司 | Method for preparing polymer anti-counterfeiting film based on nano-cellulose photonic crystal fragments |
| CN113150315A (en) * | 2021-02-26 | 2021-07-23 | 武汉大学 | Stress response type optical hydrogel and preparation method and application thereof |
| 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 |
| CN114350002A (en) * | 2022-01-08 | 2022-04-15 | 北京大学 | Deformation reconfigurable liquid crystal polymer film driver and preparation method thereof |
| CN114350002B (en) * | 2022-01-08 | 2022-09-20 | 北京大学 | Deformation reconfigurable liquid crystal polymer film driver and preparation method thereof |
| CN114702731A (en) * | 2022-04-13 | 2022-07-05 | 烟台先进材料与绿色制造山东省实验室 | Photonic crystal thin film material, preparation method thereof and application thereof in rapid visual mixed solvent identification |
| CN114702731B (en) * | 2022-04-13 | 2023-03-10 | 烟台先进材料与绿色制造山东省实验室 | Photonic crystal thin film material, preparation method thereof and application thereof in rapid visual mixed solvent identification |
| CN114621476A (en) * | 2022-04-22 | 2022-06-14 | 广东工业大学 | PH and temperature dual-stimulus responsive structural color film, preparation method thereof and application thereof in optical anti-counterfeiting |
| CN114700055A (en) * | 2022-06-07 | 2022-07-05 | 江苏集萃智能液晶科技有限公司 | Chromatography medium and chromatography device |
| CN114700055B (en) * | 2022-06-07 | 2022-09-16 | 江苏集萃智能液晶科技有限公司 | Chromatography medium and chromatography device |
| WO2023236488A1 (en) * | 2022-06-07 | 2023-12-14 | 江苏集萃智能液晶科技有限公司 | Chromatography medium and chromatography device |
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