CN103937187A - Cellulose nanocrystal enhanced flexible nanocomposite film made of polycarbonate extracted from waste optical disc and preparation method of flexible nanocomposite film - Google Patents
Cellulose nanocrystal enhanced flexible nanocomposite film made of polycarbonate extracted from waste optical disc and preparation method of flexible nanocomposite film Download PDFInfo
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- CN103937187A CN103937187A CN201410158470.0A CN201410158470A CN103937187A CN 103937187 A CN103937187 A CN 103937187A CN 201410158470 A CN201410158470 A CN 201410158470A CN 103937187 A CN103937187 A CN 103937187A
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention relates to a cellulose nanocrystal enhanced flexible nanocomposite film made of polycarbonate extracted from a waste optical disc and a preparation method of the flexible nanocomposite film. The method comprises the steps of (1) adding a cellulose raw material into a citric acid and hydrochloric acid mixed solution, reacting at the temperature of 60-100 DEG C for 1-12h, after the reaction is ended, adding an alkaline liquid to regulate the pH value to be neutral, centrifuging and carrying out freeze drying to obtain a surface functionalized cellulose nanocrystal; (2) cutting the waste optical disc into pieces, adding chloroform to stir for 1-18h, carrying out suction filtration on the mixture, and drying the filtrate to obtain polycarbonate; (3) sufficiently dissolving and uniformly mixing polycarbonate and the surface functionalized cellulose nanocrystal in an organic solvent, then, coating, and carrying out vacuum dry on the product until the product is up to the constant weight to obtain the cellulose nanocrystal enhanced flexible nanocomposite film. The preparation method provided by the invention is simple and rapid in process, cheap, efficient and suitable for industrial mass production. The obtained flexible nanocomposite film is excellent in mechanical and thermal performances, remarkably increased in refractive index and rather wide in application prospect in high-performance optical devices and particularly flexible screen materials.
Description
technical field
The invention belongs to Multifunction nano composite membrane and preparation field thereof, particularly relate to the nanocrystalline enhancing abandoned optical discs of a kind of Mierocrystalline cellulose and extract flexible compound film of polycarbonate and preparation method thereof.
background technology
Flexible display screen is also called " Electronic Paper ", be by soft material make, the flexible display unit of changeable type.Due to its reduce power consumption, light, the feature of installation and convenient transportation, is just extensively studied, and applies to portable electric appts, and pen and touch input wait equipment.Supreme Being people, film company of Du Pont announce that in 2012 the PEN of the said firm (PEN) film " Teonex " is used as circuit base material in 7.4 inches of flexible OLED display screens of Yi U.S. flexible display center exploitation.2013, Samsung was released flexible OLED screen YOUM, wherein with film membrane, had replaced the glass substrate of conventional screen.General mylar film transmittance is 90%, and resistance toheat is not high, and second-order transition temperature is 78 ℃ of left and right, and water-absorbent is larger, and PEN makes up to some extent aspect thermal characteristics, and second-order transition temperature reaches 120 ℃, but expensive.Common pure polycarbonate membrane is high temperature resistant reaches 110～130 ℃, transmittance >90%, and mist degree <0.2%, but mechanical property and thermotolerance are not fine, particularly, in the application of display screen, specific refractory power neither be very high.And polycarbonate with low cost (PC) is carried out after suitable modification, be expected to as the PEN film sheet glass that replace in traditional display screen the same as film membrane, be applied as the substrate of flexible display screen.
At present, domestic processing be take abandoned optical discs that PC is main raw material and is adopted more and burn and the traditional treatment method of landfill, but such method is not suitable for the disposal of abandoned optical discs very much: during CD burning disposal, cracking can occur, discharge even carcinogenic substance of a large amount of obnoxious flavoures, landfill process been has not only has been occupied limited arable land, and CD hard degradation, the heavy metal contamination soil that it contains, soil is poisoned, wasted a large amount of metals and polycarbonate resource.Thus, also reported the method that adopts multiple organic solvent and chemical reagent layering to recycle CD both at home and abroad, to reclaim metal and dyestuff wherein, and the complete depolymerization of the PC in CD is obtained to dihydroxyphenyl propane and methylcarbonate, method is complicated, complex steps, and cost is very high.Therefore, find a kind of simple method directly abandoned optical discs be recycled into PC material and prepare novel PC matrix material, not only helpful to the recycling of waste disk and a series of environment and the resource problem that bring, also can be applied to the such high-tech area of flexible display screen, this will be that everybody is desired.
Mierocrystalline cellulose nanocrystalline (CNC) is as one of biopolymer wild phase, and specific surface area is very large, has very high activity and surface energy, and has excellent mechanical property and biological degradability, can change significantly the performance of polymkeric substance.In recent years, the research that by physical method, Mierocrystalline cellulose nanocomposite is entered to the nano-complex that obtains excellent performance in polymeric matrix is constantly being carried out, some polymkeric substance have successfully been strengthened, as polyvinyl chloride (PVC), polypropylene (PP), polyoxyethylene (POE) etc.Donghua University once had the research of the nanocrystalline PC of being added to of Mierocrystalline cellulose [Xu W, Qin Z, Yu H, Liu Y, Liu N, Zhou Z, Chen L. Cellulose nanocrystals as organic nanofillers for transparent polycarbonate films. J Nanopart Res (2013) 15:1562-1570], on polycarbonate molecular chain, there is a large amount of ester groups, Mierocrystalline cellulose nanocrystal surface has a lot of carboxyls, between the two, produce strong hydrogen bond action, improved some performances of PC.But its Mierocrystalline cellulose using is nanocrystalline is prepared by sulfuric acid process, and residual sulfur acid group can make the thermotolerance variation of CNC, simultaneously, due to wetting ability hydroxyl and hydrophobicity PC consistency bad, so CNC addition is low, in addition, because surface is with sulfate radical, be unfavorable for improving its calorifics thermostability.
summary of the invention
The invention provides a kind of Mierocrystalline cellulose nanocrystalline (CNC) and strengthen flexible nano composite membrane of abandoned optical discs extraction polycarbonate (PC) and preparation method thereof, technique simple and fast, Cheap highly effective, be applicable to industrialized mass production.Its preparation method comprises: (1) joins cellulosic material in the mixed acid solution of citric acid and hydrochloric acid, in 60-100 ℃ of reaction 1-12h, after question response finishes, add alkali lye to be adjusted to neutrality, after centrifugal, lyophilize, obtain surface-functionalized Mierocrystalline cellulose nanocrystalline; (2) waste disk is shredded, add chloroform to stir 1-18h, then by mixture suction filtration, get after filtrate is put into vacuum drying oven oven dry and can obtain polycarbonate; (3) film after fully dissolving in organic solvent, mixing polycarbonate and surface-functionalized Mierocrystalline cellulose are nanocrystalline, product vacuum-drying is to constant weight and get final product.
In described step (1), cellulosic material is one or more in flaxen fiber, stalk fibre, Microcrystalline Cellulose, cotton, bamboo fibers, wood pulp cellulose.
In described step (1), the citric acid concentration using while configuring the mixed acid solution of described citric acid and hydrochloric acid is 3mol/L, and the concentration of hydrochloric acid is 6mol/L, and the volume ratio of citric acid and hydrochloric acid is 9:1.
In described step (1), the solid-to-liquid ratio of cellulosic material and described mixed acid solution is 1:10-90g/mL.
In described step (1), alkali lye is a kind of in sodium hydroxide solution, potassium hydroxide solution, aqua calcis, barium hydroxide solution, sodium carbonate solution, ammoniacal liquor, sodium hydrogen carbonate solution and solution of potassium carbonate, and concentration is at 0.1-6mol/L.
In described step (1), surface-functionalized Mierocrystalline cellulose is nanocrystalline is bar-shaped or ellipticity, and its particle diameter is 10-200nm, and its surface group is ester group, carboxyl or hydroxyl.
In described step (2), described waste disk is waste and old CD, DVD, LD or BD containing polycarbonate.
In described step (3), in composite membrane, the nanocrystalline massfraction of Mierocrystalline cellulose is 1-25%.
In described step (3), described organic solvent is a kind of in toluene, chloroform, tetrahydrofuran (THF), methylene dichloride and ethyl acetate.
In described step (3), the thickness of described composite membrane is 50nm-10mm.
The resulting multifunction flexible composite membrane of aforesaid method according to the present invention, mechanics and thermal property are excellent.Refractive index 1.5000 left and right of the glass of using in general display screen, optically widely used bevelled mirror is 1.6435, compares with these two kinds of optics, composite membrane refractive index of the present invention significantly improves, and can reach 1.69.This composite membrane has excellent mechanics and thermal property simultaneously, so its application prospect in high-performance optical device is very wide, for society brings huge economic benefit, realizes the recycling of waste resource simultaneously.
Beneficial effect
(1) in the preparation method of flexible nano composite membrane provided by the invention, it is nanocrystalline that the mixed acid solution of employing citric acid and hydrochloric acid is prepared Mierocrystalline cellulose, makes it not contain acid group group, do not affect the thermotolerance of CNC, and with hydrophobic group, be conducive to improve the consistency of itself and PC.
(2) in the preparation method of flexible nano composite membrane provided by the invention, adopt simple physical method from abandoned optical discs, to extract polycarbonate with chloroform, easy to operate, being applicable to scale operation uses, environment, without any pollution, is compared and will be brought huge social benefit with traditional abandoned optical discs treatment process.
(3), in the flexible nano composite membrane that prepared by the present invention, Mierocrystalline cellulose is nanocrystalline to be dispersed in polycarbonate film, agglomeration a little less than.
(4) the flexible nano composite membrane product that prepared by the present invention has good mechanical property and thermostability, and most degradation speed maximum temperature can improve more than 50 ℃, and tensile strength maximum can improve more than 70%; When CNC content reaches 8wt%, the transmitance of laminated film declines and still to remain in 10%, but specific refractory power will further reach more than 1.65, has potential application prospect in high-performance optical device, can be used as flexible display screen for electronic industry.
(5) simply controlled, the quickness and high efficiency of whole preparation process of the present invention, raw material sources are extensive, and without special, expensive equipment, are suitable for industrial mass production.
accompanying drawing explanation
Fig. 1 is the photo figure of abandoned optical discs polycarbonate-base flexible nano composite membrane and the FE-SEM of film Cross Section Morphology figure thereof.
embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Bamboo fibers raw material is joined in the nitration mixture aqueous solution of citric acid and hydrochloric acid, wherein the solid-to-liquid ratio of bamboo fibers and the nitration mixture aqueous solution is 1:50 g/mL, in 80 ℃ of reaction 6h, after question response finishes, add the ammoniacal liquor of 3mol/L to regulate PH to neutral, after centrifugal, lyophilize, obtain Mierocrystalline cellulose nanocrystalline; Waste and old CD CD is shredded, add chloroform, stir 10h, by the mixture suction filtration making, get after filtrate is put into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in to chloroform, the nanocrystalline suspension of the Mierocrystalline cellulose ultrasonic dispersion in ice-water bath that is 1% by massfraction, and both are mixed, are coated with and are taped against on slide glass, product vacuum drying obtains nano compound film, plastic film mulch thickness 0.25mm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), nanocrystalline good being dispersed in PC matrix of Mierocrystalline cellulose, and material is through properties test, compare with pure PC, the transmitance of film declines in 10%, specific refractory power has risen to 1.611 by 1.597 of PC, and tensile strength increases 13%, most degradation speed temperature (T
max) improved 10.2 ℃.This mould material has very good thermal stability and physical property, and comparatively desirable specific refractory power, has broad application prospects.
Embodiment 2
Wood pulp cellulose raw material is joined in the nitration mixture aqueous solution of citric acid and hydrochloric acid, wherein the solid-to-liquid ratio of wood pulp cellulose and the nitration mixture aqueous solution is 1:60 g/mL, in 80 ℃ of reaction 6h, after question response finishes, add the ammoniacal liquor of 1mol/L to regulate PH to neutral, after centrifugal, lyophilize, obtain Mierocrystalline cellulose nanocrystalline; Waste and old DVD CD is shredded, add chloroform, stir 10h, by the mixture suction filtration making, get after filtrate is put into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in to ethyl acetate, the nanocrystalline suspension of the Mierocrystalline cellulose ultrasonic dispersion in ice-water bath that is 8% by massfraction, and both are mixed, are coated with and are taped against on slide glass, product vacuum drying obtains nano compound film, plastic film mulch thickness 100nm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), nanocrystalline good being dispersed in PC matrix of Mierocrystalline cellulose, and material is through properties test, compare with pure PC, the transmitance of film declines in 10%, specific refractory power has risen to 1.653 by 1.597 of PC, and tensile strength increases 24%, most degradation speed temperature (T
max) improved 17.4 ℃.This mould material has very good thermal stability and physical property, and comparatively desirable specific refractory power, has broad application prospects.
Embodiment 3
Wood pulp cellulose raw material is joined in the nitration mixture aqueous solution of citric acid and hydrochloric acid, wherein the solid-to-liquid ratio of wood pulp cellulose and the nitration mixture aqueous solution is 1:70 g/mL, in 85 ℃ of reaction 7h, after question response finishes, add the sodium hydroxide solution of 2mol/L to regulate PH to neutral, after centrifugal, lyophilize, obtain Mierocrystalline cellulose nanocrystalline; Waste and old LD CD is shredded, add toluene, stir 5h, by the mixture suction filtration making, get after filtrate is put into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in to chloroform, the nanocrystalline suspension of the Mierocrystalline cellulose ultrasonic dispersion in ice-water bath that is 3% by massfraction, and both are mixed, are coated with and are taped against on slide glass, product vacuum drying obtains nano compound film, plastic film mulch thickness 6mm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), nanocrystalline good being dispersed in PC matrix of Mierocrystalline cellulose, and material is through properties test, compare with pure PC, the transmitance of film declines in 10%, specific refractory power has risen to 1.685 by 1.597 of PC, and tensile strength increases 26%, most degradation speed temperature (T
max) improved 18.1 ℃.This mould material has very good thermal stability and physical property, and comparatively desirable specific refractory power, has broad application prospects.
Embodiment 4
Fibrilia raw material is joined in the nitration mixture aqueous solution of citric acid and hydrochloric acid, wherein the solid-to-liquid ratio of wood pulp cellulose and the nitration mixture aqueous solution is 1:60 g/mL, in 75 ℃ of reaction 7h, after question response finishes, add the potassium hydroxide of 1.5mol/L to regulate PH to neutral, after centrifugal, lyophilize, obtain Mierocrystalline cellulose nanocrystalline; Waste and old CD CD is shredded, add chloroform, stir 6h, by the mixture suction filtration making, get after filtrate is put into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in to methylene dichloride, the nanocrystalline suspension of the Mierocrystalline cellulose ultrasonic dispersion in ice-water bath that is 25% by massfraction, and both are mixed, are coated with and are taped against on slide glass, product vacuum drying obtains nano compound film, plastic film mulch thickness 0.08mm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), nanocrystalline good being dispersed in PC matrix of Mierocrystalline cellulose, and material is through properties test, compare with pure PC, the transmitance of film declines in 10%, specific refractory power has risen to 1.691 by 1.597 of PC, and tensile strength increases 70%, most degradation speed temperature (T
max) improved 52.6 ℃.This mould material has very good thermal stability and physical property, and comparatively desirable specific refractory power, has broad application prospects.
Embodiment 5
Fibrilia raw material is joined in the nitration mixture aqueous solution of citric acid and hydrochloric acid, wherein the solid-to-liquid ratio of wood pulp cellulose and the nitration mixture aqueous solution is 1:20 g/mL, in 83 ℃ of reaction 9h, after question response finishes, add the barium hydroxide solution of 1mol/L to regulate PH to neutral, after centrifugal, lyophilize, obtain Mierocrystalline cellulose nanocrystalline; Waste and old BD CD is shredded, add chloroform, stir 6h, by the mixture suction filtration making, get after filtrate is put into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in to tetrahydrofuran (THF), the nanocrystalline suspension of the Mierocrystalline cellulose ultrasonic dispersion in ice-water bath that is 18% by massfraction, and both are mixed, are coated with and are taped against on slide glass, product vacuum drying obtains nano compound film, plastic film mulch thickness 2000nm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), nanocrystalline good being dispersed in PC matrix of Mierocrystalline cellulose, and material is through properties test, compare with pure PC, the transmitance of film declines in 10%, specific refractory power has risen to 1.670 by 1.597 of PC, and tensile strength increases 46%, most degradation speed temperature (T
max) improved 30.7 ℃.This mould material has very good thermal stability and physical property, and comparatively desirable specific refractory power, has broad application prospects.
Claims (10)
1. the nanocrystalline enhancing abandoned optical discs of a Mierocrystalline cellulose extracts the preparation method of the flexible nano composite membrane of polycarbonate, described method comprises: (1) joins cellulosic material in the mixed acid solution of citric acid and hydrochloric acid, in 60-100 ℃ of reaction 1-12h, after question response finishes, add alkali lye to be adjusted to neutrality, after centrifugal, lyophilize, obtain surface-functionalized Mierocrystalline cellulose nanocrystalline; (2) waste disk is shredded, add chloroform to stir 1-18h, then by mixture suction filtration, get after filtrate is put into vacuum drying oven oven dry and obtain polycarbonate; (3) film after fully dissolving in organic solvent, mixing polycarbonate and surface-functionalized Mierocrystalline cellulose are nanocrystalline, product vacuum-drying to constant weight obtains flexible nano composite membrane.
2. the nanocrystalline enhancing abandoned optical discs of a kind of Mierocrystalline cellulose according to claim 1 extracts the preparation method of the flexible nano composite membrane of polycarbonate, it is characterized in that: in step (1), described cellulosic material is one or more in flaxen fiber, stalk fibre, Microcrystalline Cellulose, cotton, bamboo fibers, wood pulp cellulose.
3. the nanocrystalline enhancing abandoned optical discs of a kind of Mierocrystalline cellulose according to claim 1 extracts the preparation method of the flexible nano composite membrane of polycarbonate, it is characterized in that: in step (1), the solid-to-liquid ratio of described cellulosic material and described mixed acid solution is 1:10-90g/mL.
4. the nanocrystalline enhancing abandoned optical discs of a kind of Mierocrystalline cellulose according to claim 1 extracts the preparation method of the flexible nano composite membrane of polycarbonate, it is characterized in that: in step (1), the citric acid concentration using while configuring the mixed acid solution of described citric acid and hydrochloric acid is 3mol/L, the concentration of hydrochloric acid is 6mol/L, and the volume ratio of citric acid and hydrochloric acid is 9:1.
5. the nanocrystalline enhancing abandoned optical discs of a kind of Mierocrystalline cellulose according to claim 1 extracts the preparation method of the flexible nano composite membrane of polycarbonate, it is characterized in that: in step (1), described alkali lye is a kind of in sodium hydroxide solution, potassium hydroxide solution, aqua calcis, barium hydroxide solution, sodium carbonate solution, ammoniacal liquor, sodium hydrogen carbonate solution and solution of potassium carbonate, and concentration is at 0.1-6mol/L.
6. the nanocrystalline enhancing abandoned optical discs of a kind of Mierocrystalline cellulose according to claim 1 extracts the preparation method of the flexible nano composite membrane of polycarbonate, it is characterized in that: in step (1), described surface-functionalized Mierocrystalline cellulose is nanocrystalline is bar-shaped or ellipticity, its particle diameter is 10-200nm, and its surface group is ester group, carboxyl or hydroxyl.
7. the nanocrystalline enhancing abandoned optical discs of a kind of Mierocrystalline cellulose according to claim 1 extracts the preparation method of the flexible nano composite membrane of polycarbonate, it is characterized in that: in step (2), described waste disk is waste and old CD, DVD, LD or BD containing polycarbonate.
8. the nanocrystalline enhancing abandoned optical discs of a kind of Mierocrystalline cellulose according to claim 1 extracts the preparation method of the flexible nano composite membrane of polycarbonate, it is characterized in that: in step (3), in described composite membrane, the nanocrystalline massfraction of Mierocrystalline cellulose is 1-25%, and described organic solvent is a kind of in toluene, chloroform, tetrahydrofuran (THF), methylene dichloride and ethyl acetate.
9. the nanocrystalline enhancing abandoned optical discs of a kind of Mierocrystalline cellulose according to claim 1 extracts the preparation method of the flexible nano composite membrane of polycarbonate, it is characterized in that: the thickness of described composite membrane is 50nm-10mm.
10. the nanocrystalline enhancing abandoned optical discs of Mierocrystalline cellulose extracts a flexible nano composite membrane for polycarbonate, and it is obtained by the method preparation described in claim 1-9 any one.
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| CN201410158470.0A CN103937187B (en) | 2014-04-21 | 2014-04-21 | A kind of Cellulose nanocrystal strengthens abandoned optical discs and extracts flexible nano composite membrane of polycarbonate and preparation method thereof |
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Cited By (4)
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| CN105366786A (en) * | 2015-12-23 | 2016-03-02 | 杭州万事利丝绸科技有限公司 | Silk printing and dyeing wastewater treatment process based on cellulose flocculant |
| CN107353400A (en) * | 2017-07-13 | 2017-11-17 | 华中科技大学 | A kind of preparation method of polypropylene carbonate/Cellulose nanocrystal composite |
| CN107446322A (en) * | 2017-06-27 | 2017-12-08 | 鲍亚盟 | A kind of less than 50 microns optical film plastic basis materials and preparation method thereof |
| CN112679762A (en) * | 2020-12-14 | 2021-04-20 | 苏州博利迈新材料科技有限公司 | Preparation method of high-fluidity fiber-reinforced PC composite material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105366786A (en) * | 2015-12-23 | 2016-03-02 | 杭州万事利丝绸科技有限公司 | Silk printing and dyeing wastewater treatment process based on cellulose flocculant |
| CN107446322A (en) * | 2017-06-27 | 2017-12-08 | 鲍亚盟 | A kind of less than 50 microns optical film plastic basis materials and preparation method thereof |
| CN107353400A (en) * | 2017-07-13 | 2017-11-17 | 华中科技大学 | A kind of preparation method of polypropylene carbonate/Cellulose nanocrystal composite |
| CN107353400B (en) * | 2017-07-13 | 2019-02-01 | 华中科技大学 | A kind of preparation method of polypropylene carbonate/Cellulose nanocrystal composite material |
| CN112679762A (en) * | 2020-12-14 | 2021-04-20 | 苏州博利迈新材料科技有限公司 | Preparation method of high-fluidity fiber-reinforced PC composite material |
| CN112679762B (en) * | 2020-12-14 | 2023-06-02 | 苏州博利迈新材料科技有限公司 | Preparation method of high-fluidity fiber reinforced PC composite material |
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