CN106590179A - CNC/PEG composite coating and preparation method thereof - Google Patents
CNC/PEG composite coating and preparation method thereof Download PDFInfo
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- CN106590179A CN106590179A CN201610913213.2A CN201610913213A CN106590179A CN 106590179 A CN106590179 A CN 106590179A CN 201610913213 A CN201610913213 A CN 201610913213A CN 106590179 A CN106590179 A CN 106590179A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
- C09D101/02—Cellulose; Modified cellulose
- C09D101/04—Oxycellulose; Hydrocellulose
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a CNC/PEG composite coating. The CNC/PEG composite coating contains cellulose nanocrystals and polyethylene glycol, wherein the polyethylene glycol accounts for 0-50% of the mass percentage content of the cellulose nanocrystals, the particle length dimension of the cellulose nanocrystals is 151-167 nm, and the diameter is 48-52 nm. The invention further discloses a preparation method of the CNC/PEG composite coating. Natural cellulose is utilized as a raw material, the non-toxic and pollution-free PEG is utilized as a coating color regulator and a plasticizer, the prepared colorful coating is environmentally friendly and is degradable, the mechanical properties are greatly improved, and a structural color is bright and can be adjusted and controlled. In addition, the coating can be prepared through blending and compounding and dropwise simple coating on the surface of a base material, the preparation process is simple and easy to control, and the cost is low.
Description
Technical field
The invention belongs to coatings art, and in particular to a kind of CNC/PEG composite coatings and preparation method thereof.
Background technology
The method that conventional preparation has color coating is obtained by chemical reaction, such as by inorganic salt and Hard Fat
Sour sodium reaction, or the fluorine-containing nitrogen dyestuff of grafting, these methods can produce many pollution problems, and preparation cost is higher；And
At present typical commercial polyurethane class coating, the organic solvent content height used by it, can cause serious VOC to pollute；Existing skill
The color of the color coating in art is single unadjustable.
Cellulose nanocrystal is a kind of new liquid crystal material of cholesteric phase, and crystal can occur in higher concentrations anisotropy to respectively
To the same sex, the transformation until forming liquid crystalline phase.Cellulose nanocrystal light weight, excellent in mechanical performance, light transmission it is good, good from group
Dress performance so as to there is huge application potential in the high-end technical field such as liquid crystal material, precision optics, medical material.
The at present both at home and abroad application to Cellulose nanocrystal in coating is rarely reported, and this liquid crystal coatings have high-crystallinity and regular
Structural arrangement, with bright-coloured bright and beautiful structural color, and can not be replicated by common pigments, if this coating internal structure row
Row be not modified, then this structural color can long sustaining, the problems such as colour fading without common pigments, this more conforms to modern society's energy-conservation
The theory of environmental protection so as to have widely application at aspects such as building material surface decoration, anti-counterfeiting marks.
The content of the invention
Goal of the invention：The invention aims to the color for solving color coating in prior art it is single it is unadjustable,
With the problems such as environmental pollution, there is provided a kind of composite coating of environment-friendly degradable, and Color tunable.
Technical scheme：A kind of CNC/PEG composite coatings, including Cellulose nanocrystal and Polyethylene Glycol, Polyethylene Glycol accounts for fibre
The nanocrystalline weight/mass percentage composition of dimension element is 0～50%, and the particle size length of the Cellulose nanocrystal is 151～167nm,
A diameter of 48-52nm.
A kind of preparation method of CNC/PEG composite coatings, including following several steps：
1) preparation of Cellulose nanocrystal (CNC) suspension：Cellulose is prepared using the method for sulphuric acid hydrolysis cellulose to receive
Rice crystalline suspension liquid；The preparation method uses prior art, will not be described here；
2) preparation of Polyethylene Glycol (PEG) solution：Polyethylene Glycol is dissolved in water, polyglycol solution is obtained；
3) polyglycol solution in step (2) is added dropwise in the Cellulose nanocrystal suspension in step (1), is stirred
Mix homogeneously, obtains CNC/PEG composite suspension liquid；By CNC/PEG composite suspension liquid evaporation and concentration, then deaeration process is carried out, obtained
To CNC/PEG composite coating stock solutions.
Further, the step 3) in be uniformly mixed after carry out supersound process in ultrasonic washing instrument again；Institute
The ultrasonic power for stating supersound process is 200W, ultrasonic time 2min.
Cellulose nanocrystal has the characteristics such as high-crystallinity, high elastic modulus, high intensity, due to its too high cohesiveness,
Adhesion Dipeptiven between the nanocrystalline coloured coating of pure cellulose and common plastic substrates is low.And the amphiphilic macromolecular such as PEG has very
Good plasticising performance, therefore, using Cellulose nanocrystal as host matrix, the high molecular polymers such as PEG are combined, retain cellulose
While nanocrystalline liquid crystal characteristic, can also improve its mechanical property, expand its application in coatings art.
CNC/PEG coatings designed by the present invention can be coated on various plastic plates, such as POM, PC, ABS, PA plastics
Plate.
The present invention compared with prior art, has the advantage that：The present invention by the use of native cellulose as raw material, using nothing
The free of contamination PEG of poison is used as coating color regulator and plasticizer, the coloured coating environment-friendly degradable for preparing, mechanical performance
Substantially improved, and the bright-coloured controllable of structural color；On the other hand, by composite, simple drop coating is in substrate surface
Can be obtained, preparation process is simple, easily controllable, low cost.
Description of the drawings
Fig. 1 is the micropolariscope photo of CNC/PEG composite coating films in the embodiment of the present invention 1；
Fig. 2 is the SEM photograph of CNC/PEG composite coating films cross section in the embodiment of the present invention 1；
Fig. 3 is the tensile property test of obtained CNC/PEG composite coatings film in the embodiment of the present invention；
Fig. 4 is coated in the adhesion test of the CNC/PEG composite coatings on ABS plates for the embodiment of the present invention.
Specific embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, this
A little embodiments are only used for the explanation present invention, do not constitute limiting the scope of the present invention.
Embodiment 1
1) preparation of Cellulose nanocrystal suspension：4.0g Microcrystalline Cellulose is mixed with 80ml concentration for 64wt% sulphuric acid
Close, after mechanical agitation 2h in 50 DEG C of water-baths, the distilled water for adding 5 times of amounts stops hydrolysis, and the suspension after dilution falls
Enter bag filter, dialyse in distilled water several days and remove unnecessary acid, the saccharide of small-molecular-weight, and other water-solubility impurities；
It is about the 6.0 nanocrystalline CNC suspensions of aqueous fiber element to pH value, concentration is 0.5wt%.(herein Cellulose nanocrystal suspends
The list of references of liquid and preparation method thereof is Liu, D.；Wang,S；Ma,Z.；Tian,D.；Gu,M.；Lin,F.Structure-color
mechanism of iridescent cellulose nanocrystal films.RSC Adv.2014,4,39322-
39331.)
2) prepared by PEG solution：5gPEG20000 is dispersed in 100ml distilled water, after stirring makes it fully dissolve, is stood
The bubble gone out in system, obtains PEG solution concentrations for 5%.
3) preparation of CNC/PEG composite coatings：0.25ml concentration is added separately to into 50ml celluloses for 5%PEG solution
In nanocrystal suspension, stirring and supersound process 2min under 200W power in ultrasonic washing instrument are obtained after mix homogeneously
CNC/PEG composite suspension liquid；CNC/PEG composite suspensions liquid is evaporated at ambient conditions concentration, then carries out deaeration process,
Obtain the CNC/PEG composite coating stock solutions that concentration is 2wt%.
Embodiment 2
The present embodiment is step 3 with the difference of embodiment 1), 0.5ml concentration is separately added into for 5%PEG solution
To in 50ml Cellulose nanocrystal suspensions, stir and supersound process 2min, the mixing under 200W power in ultrasonic washing instrument
CNC/PEG composite suspension liquid is obtained after uniform；CNC/PEG composite suspensions liquid is evaporated at ambient conditions concentration, then is entered
Row deaeration is processed, and obtains CNC/PEG composite coating stock solutions.
Embodiment 3
The present embodiment is step 3 with the difference of embodiment 1), 0.75ml concentration is added respectively for 5%PEG solution
Enter in 50ml Cellulose nanocrystal suspensions, stirring and supersound process 2min under 200W power in ultrasonic washing instrument are mixed
CNC/PEG composite suspension liquid is obtained after closing uniformly；CNC/PEG composite suspensions liquid is evaporated at ambient conditions concentration, then
Deaeration process is carried out, CNC/PEG composite coating stock solutions are obtained.
Embodiment 4
The present embodiment is step 3 with the difference of embodiment 1), 1.0ml concentration is separately added into for 5%PEG solution
To in 50ml Cellulose nanocrystal suspensions, stir and supersound process 2min, the mixing under 200W power in ultrasonic washing instrument
CNC/PEG composite suspension liquid is obtained after uniform；CNC/PEG composite suspensions liquid is evaporated at ambient conditions concentration, then is entered
Row deaeration is processed, and obtains CNC/PEG composite coating stock solutions.
Embodiment 5
The present embodiment is step 3 with the difference of embodiment 1), 1.5ml concentration is separately added into for 5%PEG solution
To in 50ml Cellulose nanocrystal suspensions, stir and supersound process 2min, the mixing under 200W power in ultrasonic washing instrument
CNC/PEG composite suspension liquid is obtained after uniform；CNC/PEG composite suspensions liquid is evaporated at ambient conditions concentration, then is entered
Row deaeration is processed, and obtains CNC/PEG composite coating stock solutions.
Embodiment 6
The present embodiment is step 3 with the difference of embodiment 1), 2.0ml concentration is separately added into for 5%PEG solution
To in 50ml Cellulose nanocrystal suspensions, stir and supersound process 2min, the mixing under 200W power in ultrasonic washing instrument
CNC/PEG composite suspension liquid is obtained after uniform；CNC/PEG composite suspensions liquid is evaporated at ambient conditions concentration, then is entered
Row deaeration is processed, and obtains CNC/PEG composite coating stock solutions.
Embodiment 7
The present embodiment is step 3 with the difference of embodiment 1), 2.5ml concentration is separately added into for 5%PEG solution
To in 50ml Cellulose nanocrystal suspensions, stir and supersound process 2min, the mixing under 200W power in ultrasonic washing instrument
CNC/PEG composite suspension liquid is obtained after uniform；CNC/PEG composite suspensions liquid is evaporated at ambient conditions concentration, then is entered
Row deaeration is processed, and obtains CNC/PEG composite coating stock solutions.
The preparation of pure CNC coated film：
The preparation of Cellulose nanocrystal suspension：4.0g Microcrystalline Cellulose is mixed with 80ml concentration for 64wt% sulphuric acid,
After mechanical agitation 2h in 50 DEG C of water-baths, the distilled water for adding 5 times of amounts stops hydrolysis, and the suspension after dilution is poured into
Analysis bag, dialyses several days in distilled water and removes unnecessary acid, the saccharide of small-molecular-weight, and other water-solubility impurities；Obtain pH
The nanocrystalline CNC suspensions of aqueous fiber element of value about 6.0, concentration is 0.5wt%.By CNC composite suspension liquid in environmental condition
Under be evaporated concentration, then carry out deaeration process, obtain CNC coating stock solutions.
Performance test embodiment
Mixed CNC/PEG composite suspensions liquid in embodiment 1 is placed in the politef diaphragm capsule of a diameter of 9mm,
The CNC/PEG colour composite coating films that self-supporting can be opened are dried in 30 DEG C of baking ovens, the polarisation for obtaining composite coating film shows
Micro mirror photo is shown in that Fig. 1 and the SEM photograph of composite coating film cross section are shown in Fig. 2.
As shown in figure 1, CNC/PEG composite coating films remain the cholesteric liquid crystal structure of pure fiber nanocrystalline coating film,
It can be seen that with the increase of PEG content, fingerprint pitch constantly increases, at the same under polarizing microscope thin film color also changing,
It is changed into orange from blueness；Fig. 2 is visible, is a layer structure inside pure cellulose nanocrystalline coating film, and the addition of PEG retains
Layer structure, while increase distance between layers.But when the PEG content for adding is too high, after 30%, due to
PEG assembles in system, and the cholesteric liquid crystal of Cellulose nanocrystal is destructurized, and coated film color is thin out or even disappears
Lose.The maximum reflection wavelength that ultraviolet spectra testing result pure cellulose nanocrystalline coating film is measured be 425nm, CNC/PEG2.5,
CNC/PEG5, CNC/PEG7.5, CNC/PEG10, CNC/PEG15, CNC/PEG20, CNC/PEG30, CNC/PEG40 coated film
Maximum reflection wavelength is respectively 435nm, 442nm, 443nm, 460nm, 475nm, 481nm, 545nm, and 494nm is with PEG content
Increase (be less than 30%), integrally present a red shift.
Tensile property test is carried out to CNC/PEG composite coatings film prepared by embodiment 2,4,5,6,7, as a result such as Fig. 3 institutes
Show.Compared to pure cellulose nanocrystalline coating film, after being combined PEG and Cellulose nanocrystal in the present invention, with PEG content
Increase, the pliability of coated film substantially increases.
CNC/PEG composite coating stock solutions prepared by embodiment 1,3,4,5,6,7 are respectively coated on into ABS plastic with drop-coating
On plate, it is dried under environmental condition, adhesive force test is then carried out, as shown in figure 4, result is visible with the continuous increasing of PEG content
Plus (be less than 30%), coating is also improved constantly in the adhesive force of ABS plastic plate surface, amphiphilic due to PEG, on the one hand many
Hydroxyl structure so as to there is stronger hydrogen bond action with the hydroxyl of Cellulose nanocrystal, it is easy to be dispersed between CNC layers；Simultaneously
PEG main chains have hydrophobicity again so as to there is affinity between the plastic plate such as ABS, increased CNC/PEG coatings and ABS etc.
Adhesive force between base material.
Claims (4)
1. a kind of CNC/PEG composite coatings, it is characterised in that including Cellulose nanocrystal and Polyethylene Glycol, Polyethylene Glycol accounts for fibre
The nanocrystalline weight/mass percentage composition of dimension element is 0～50%, and the particle size length of the Cellulose nanocrystal is 151～167nm,
A diameter of 48-52nm.
2. a kind of preparation method of CNC/PEG composite coatings, it is characterised in that including following several steps：
1) preparation of Cellulose nanocrystal suspension：Cellulose nanocrystal is prepared using the method for sulphuric acid hydrolysis cellulose to suspend
Liquid；
2) preparation of polyglycol solution：Polyethylene Glycol is dissolved in water, polyglycol solution is obtained；
3) polyglycol solution in step (2) is added dropwise in the Cellulose nanocrystal suspension in step (1), stirring mixing
Uniformly, CNC/PEG composite suspension liquid is obtained；By CNC/PEG composite suspension liquid evaporation and concentration, then deaeration process is carried out, obtained
CNC/PEG composite coating stock solutions.
3. the preparation method of CNC/PEG composite coatings according to claim 2, it is characterised in that the step 3) in stir
Mix after mix homogeneously carries out again supersound process in ultrasonic washing instrument.
4. the preparation method of CNC/PEG composite coatings according to claim 3, it is characterised in that the supersound process
Ultrasonic power is 200W, ultrasonic time 2min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111944070A (en) * | 2019-05-14 | 2020-11-17 | 中国科学技术大学 | Biomass nano-composite environment-friendly water-based antibacterial coating and preparation method thereof |
| CN112759982A (en) * | 2020-12-24 | 2021-05-07 | 南京信息工程大学 | PVA/CNC composite coating and preparation method and application thereof |
| CN114904053A (en) * | 2022-05-31 | 2022-08-16 | 重庆大学 | Cellulose nanocrystal-based anti-inflammatory and anti-tissue adhesion biological coating and preparation method and application thereof |
| CN115850801A (en) * | 2022-10-21 | 2023-03-28 | 浙江理工大学 | Preparation method of humidity-driven color-variable artificial muscle based on cellulose nanocrystals |
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| CN111944070A (en) * | 2019-05-14 | 2020-11-17 | 中国科学技术大学 | Biomass nano-composite environment-friendly water-based antibacterial coating and preparation method thereof |
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| CN114904053A (en) * | 2022-05-31 | 2022-08-16 | 重庆大学 | Cellulose nanocrystal-based anti-inflammatory and anti-tissue adhesion biological coating and preparation method and application thereof |
| CN115850801A (en) * | 2022-10-21 | 2023-03-28 | 浙江理工大学 | Preparation method of humidity-driven color-variable artificial muscle based on cellulose nanocrystals |
| CN115850801B (en) * | 2022-10-21 | 2024-05-10 | 浙江理工大学 | Preparation method of humidity-driven variable color artificial muscle based on cellulose nanocrystalline |
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Effective date of registration: 20221222 Address after: No. 88-2, pubin Avenue, Jiangpu street, Pukou District, Nanjing, Jiangsu 210000 Patentee after: Nanjing ruiniu Nenghuan New Material Technology Co.,Ltd. Address before: 210044 No. 219, Ning six road, Nanjing, Jiangsu Patentee before: Nanjing University of Information Science and Technology |
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