CN103937187B - A kind of Cellulose nanocrystal strengthens abandoned optical discs and extracts flexible nano composite membrane of polycarbonate and preparation method thereof - Google Patents
A kind of Cellulose nanocrystal strengthens abandoned optical discs and extracts flexible nano composite membrane of polycarbonate and preparation method thereof Download PDFInfo
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- CN103937187B CN103937187B CN201410158470.0A CN201410158470A CN103937187B CN 103937187 B CN103937187 B CN 103937187B CN 201410158470 A CN201410158470 A CN 201410158470A CN 103937187 B CN103937187 B CN 103937187B
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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
- 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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- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The present invention relates to a kind of Cellulose nanocrystal and strengthen flexible nano composite membrane of abandoned optical discs extraction polycarbonate and preparation method thereof, the method comprises: 1) added by cellulosic material in the mixed acid solution of citric acid and hydrochloric acid, in 60-100 DEG C of reaction 1-12h, question response terminates to add alkali lye and is adjusted to neutrality, after centrifugal, lyophilize, obtain surface-functionalized Cellulose nanocrystal; 2) waste disk is shredded, adds chloroform and stir 1-18h, then by mixture suction filtration, get filtrate dry after polycarbonate; 3) fully dissolved in organic solvent with surface-functionalized Cellulose nanocrystal by polycarbonate, mix rear film, product vacuum is dried to constant weight and get final product.Present invention process simple and fast, Cheap highly effective, be applicable to industrialized mass production.The flexible nano composite membrane mechanics of gained and thermal property are excellent, and refractive index significantly improves, in high performance optics, particularly have very strong application prospect in flexible screen material.
Description
Technical field
The invention belongs to Multifunction nano composite membrane and preparation field thereof, particularly relate to a kind of Cellulose nanocrystal and strengthen flexible compound film of abandoned optical discs extraction polycarbonate and preparation method thereof.
Background technology
Flexible display screen is also called " Electronic Paper ", be made up of the material of softness, 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, DuPont Film company announce that in 2012 PEN (PEN) film " Teonex " of the said firm is used as circuit base material in 7.4 inch flexible OLED display screen of U.S.'s flexible display center exploitation.2013, Samsung was proposed flexible OLED screen curtain YOUM, wherein instead of the glass substrate of conventional screen with film membrane.General mylar film transmittance is 90%, and resistance toheat is not high, and second-order transition temperature is at about 78 DEG C, and water-absorbent is comparatively large, and PEN then makes up to some extent in thermal characteristics, and second-order transition temperature reaches 120 DEG C, but expensive.Common pure polycarbonate membrane is high temperature resistant reaches 110 ~ 130 DEG C, transmittance >90%, mist degree <0.2%, but mechanical property and thermotolerance are not fine, and particularly in the application of display screen, specific refractory power neither be very high.And polycarbonate (PC) with low cost is carried out suitably modified, 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 process take PC as the abandoned optical discs of the main raw material traditional treatment method adopting burning and landfill more, but such method is not suitable for the disposal of abandoned optical discs very much: cracking can occur during CD burning disposal, discharge a large amount of obnoxious flavoures even carcinogenic substance, landfill stabilization method has has not only occupied limited arable land, and CD is difficult to degraded, the heavy metal contamination soil that it contains, soil is poisoned, wastes a large amount of metal and polycarbonate resource.Thus, also report the method adopting multiple organic solvent and chemical reagent layering to recycle CD both at home and abroad, to reclaim metal wherein and dyestuff, and complete for the PC in CD depolymerization is obtained dihydroxyphenyl propane and methylcarbonate, method is complicated, and complex steps, cost is very high.Therefore, a kind of simple method is found directly abandoned optical discs to be recycled into PC material and to prepare novel PC matrix material, not only to the recycling of waste disk and a series of environment and resources problems of bringing helpful, also can be applied to the such high-tech area of flexible display screen, this will be desired by everybody.
Cellulose nanocrystal (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 the performance of polymkeric substance significantly.In recent years, the research by physical method, Cellulose nanocrystal compound being entered in polymeric matrix to obtain the nano-complex of excellent performance is constantly being carried out, successfully strengthen some polymkeric substance, as polyvinyl chloride (PVC), polypropylene (PP), polyoxyethylene (POE) etc.Once there was research [XuW Cellulose nanocrystal being added to PC in Donghua University, QinZ, YuH, LiuY, LiuN, ZhouZ, ChenL.Cellulosenanocrystalsasorganicnanofillersfortransp arentpolycarbonatefilms.JNanopartRes (2013) 15:1562-1570], polycarbonate molecular chain there is a large amount of ester groups, there is a lot of carboxyls on Cellulose nanocrystal surface, therebetween produce strong hydrogen bond action, improve some performances of PC.But its Cellulose nanocrystal used is prepared by sulfuric acid process, residual sulfur acid group can make the thermotolerance of CNC be deteriorated, simultaneously, due to hydrophilic hydroxy group and hydrophobicity PC consistency bad, therefore 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 Cellulose nanocrystal (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: cellulosic material joins in the mixed acid solution of citric acid and hydrochloric acid by (1), in 60-100 DEG C of reaction 1-12h, after question response terminates, add alkali lye and be adjusted to neutrality, after centrifugal, lyophilize, obtain surface-functionalized Cellulose nanocrystal; (2) waste disk is shredded, add chloroform and stir 1-18h, then by mixture suction filtration, get filtrate and put into after vacuum drying oven is dried and can obtain polycarbonate; (3) fully dissolved in organic solvent with surface-functionalized Cellulose nanocrystal by polycarbonate, mix rear film, product vacuum is dried 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 used when 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 the one 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 Cellulose nanocrystal 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 massfraction of Cellulose nanocrystal is 1-25%.
In described step (3), described organic solvent is the one in toluene, chloroform, tetrahydrofuran (THF), methylene dichloride and ethyl acetate.
In described step (3), the thickness of described composite membrane is 50nm-10mm.
The multifunction flexible composite membrane that aforesaid method according to the present invention obtains, mechanics and thermal property excellence.The refractive index about 1.5000 of the glass in general display screen, optically widely used bevelled mirror is 1.6435, and compared 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, and therefore its application prospect in high performance optics is very wide, simultaneously for society brings huge economic benefit, realizes the recycling of waste resource.
Beneficial effect
(1) in the preparation method of flexible nano composite membrane provided by the invention, adopt the mixed acid solution of citric acid and hydrochloric acid to prepare Cellulose nanocrystal, make it not containing sulfonate groups, do not affect the thermotolerance of CNC, and with hydrophobic group, be conducive to improving the consistency of itself and PC.
(2) in the preparation method of flexible nano composite membrane provided by the invention, simple physical method chloroform is adopted to extract polycarbonate from abandoned optical discs, easy to operate, be applicable to scale operation to use, to environment without any pollution, huge social benefit will be brought compared with traditional abandoned optical discs treatment process.
(3), in the flexible nano composite membrane that prepared by the present invention, Cellulose nanocrystal is dispersed in polycarbonate film, and agglomeration is more weak.
(4) the flexible nano composite membrane product that prepared by the present invention has good mechanical property and thermostability, and most degradation rate temperature is maximum can improve more than 50 DEG C, and tensile strength is maximum improves more than 70%; When CNC content reaches 8wt%, the transmitance of laminated film declines and still remains within 10%, but specific refractory power will reach more than 1.65 further, has potential application prospect in high performance optics, 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 the need to 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 figure of film Cross Section Morphology thereof.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
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 1:50g/mL, in 80 DEG C of reaction 6h, after question response terminates, the ammoniacal liquor adding 3mol/L regulates PH to neutral, after centrifugal, lyophilize, obtain Cellulose nanocrystal; Waste and old CD CD is shredded, adds chloroform, stir 10h, by obtained mixture suction filtration, get after filtrate puts into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in chloroform, is Cellulose nanocrystal suspension ultrasonic disperse in ice-water bath of 1% by massfraction, and both is mixed, is coated with and is taped against on slide glass, and product vacuum is dried and namely obtained nano compound film, plastic film mulch thickness 0.25mm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), what Cellulose nanocrystal was good is dispersed in PC matrix, and material is tested through properties, compared with pure PC, the transmitance of film declines within 10%, specific refractory power has risen to 1.611 by 1.597 of PC, and tensile strength increases 13%, most degradation rate temperature (T
max) improve 10.2 DEG C.This mould material has very good thermal stability and physical property, and ideal 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 1:60g/mL, in 80 DEG C of reaction 6h, after question response terminates, the ammoniacal liquor adding 1mol/L regulates PH to neutral, after centrifugal, lyophilize, obtain Cellulose nanocrystal; Waste and old DVD CD is shredded, adds chloroform, stir 10h, by obtained mixture suction filtration, get after filtrate puts into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in ethyl acetate, is Cellulose nanocrystal suspension ultrasonic disperse in ice-water bath of 8% by massfraction, and both is mixed, is coated with and is taped against on slide glass, and product vacuum is dried and namely obtained nano compound film, plastic film mulch thickness 100nm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), what Cellulose nanocrystal was good is dispersed in PC matrix, and material is tested through properties, compared with pure PC, the transmitance of film declines within 10%, specific refractory power has risen to 1.653 by 1.597 of PC, and tensile strength increases 24%, most degradation rate temperature (T
max) improve 17.4 DEG C.This mould material has very good thermal stability and physical property, and ideal 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 1:70g/mL, in 85 DEG C of reaction 7h, after question response terminates, the sodium hydroxide solution adding 2mol/L regulates PH to neutral, after centrifugal, lyophilize, obtain Cellulose nanocrystal; Waste and old LD CD is shredded, adds toluene, stir 5h, by obtained mixture suction filtration, get after filtrate puts into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in chloroform, is Cellulose nanocrystal suspension ultrasonic disperse in ice-water bath of 3% by massfraction, and both is mixed, is coated with and is taped against on slide glass, and product vacuum is dried and namely obtained nano compound film, plastic film mulch thickness 6mm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), what Cellulose nanocrystal was good is dispersed in PC matrix, and material is tested through properties, compared with pure PC, the transmitance of film declines within 10%, specific refractory power has risen to 1.685 by 1.597 of PC, and tensile strength increases 26%, most degradation rate temperature (T
max) improve 18.1 DEG C.This mould material has very good thermal stability and physical property, and ideal 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 1:60g/mL, in 75 DEG C of reaction 7h, after question response terminates, the potassium hydroxide adding 1.5mol/L regulates PH to neutral, after centrifugal, lyophilize, obtain Cellulose nanocrystal; Waste and old CD CD is shredded, adds chloroform, stir 6h, by obtained mixture suction filtration, get after filtrate puts into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in methylene dichloride, is Cellulose nanocrystal suspension ultrasonic disperse in ice-water bath of 25% by massfraction, and both is mixed, is coated with and is taped against on slide glass, and product vacuum is dried and namely obtained nano compound film, plastic film mulch thickness 0.08mm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), what Cellulose nanocrystal was good is dispersed in PC matrix, and material is tested through properties, compared with pure PC, the transmitance of film declines within 10%, specific refractory power has risen to 1.691 by 1.597 of PC, and tensile strength increases 70%, most degradation rate temperature (T
max) improve 52.6 DEG C.This mould material has very good thermal stability and physical property, and ideal 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 1:20g/mL, in 83 DEG C of reaction 9h, after question response terminates, the barium hydroxide solution adding 1mol/L regulates PH to neutral, after centrifugal, lyophilize, obtain Cellulose nanocrystal; Waste and old BD CD is shredded, adds chloroform, stir 6h, by obtained mixture suction filtration, get after filtrate puts into oven for drying and obtain polycarbonate; Polycarbonate is dissolved in tetrahydrofuran (THF), is Cellulose nanocrystal suspension ultrasonic disperse in ice-water bath of 18% by massfraction, and both is mixed, is coated with and is taped against on slide glass, and product vacuum is dried and namely obtained nano compound film, plastic film mulch thickness 2000nm.
This film Cross Section Morphology is observed through scanning electron microscope (SEM), what Cellulose nanocrystal was good is dispersed in PC matrix, and material is tested through properties, compared with pure PC, the transmitance of film declines within 10%, specific refractory power has risen to 1.670 by 1.597 of PC, and tensile strength increases 46%, most degradation rate temperature (T
max) improve 30.7 DEG C.This mould material has very good thermal stability and physical property, and ideal specific refractory power, has broad application prospects.
Claims (2)
1. a Cellulose nanocrystal strengthens the preparation method that abandoned optical discs extracts the flexible nano composite membrane of polycarbonate, its concrete steps are: fibrilia raw material joins in the nitration mixture aqueous solution of citric acid and hydrochloric acid by (1), wherein, the citric acid concentration used when preparing described mixed acid solution is 3mol/L, concentration of hydrochloric acid is 6mol/L, the volume ratio of citric acid and hydrochloric acid is 9:1, the solid-to-liquid ratio of fibrilia raw material and the nitration mixture aqueous solution is 1:60g/mL, in 75 DEG C of reaction 7h, after question response terminates, the potassium hydroxide adding 1.5mol/L regulates pH to neutral, through centrifugal, Cellulose nanocrystal is obtained after lyophilize, (2) waste and old CD CD is shredded, add chloroform, stir 6h, by obtained mixture suction filtration, get after filtrate puts into oven for drying and obtain polycarbonate, (3) polycarbonate is dissolved in methylene dichloride, be Cellulose nanocrystal suspension ultrasonic disperse in ice-water bath of 25% by massfraction, and both are mixed, be entirely coated with and be taped against on slide glass, product vacuum is dried and is namely obtained nano compound film, plastic film mulch thickness 0.08mm, compared with pure PC, film transmission rate declines within 10%, and specific refractory power rises to 1.691 by 1.597 of PC, and tensile strength increases 70%, and most degradation rate temperature improves 52.6 DEG C.
2. Cellulose nanocrystal strengthens the flexible nano composite membrane that abandoned optical discs extracts polycarbonate, and it is prepared by method according to claim 1 and obtains.
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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 |
| 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 |
| 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 |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040663A (en) * | 2010-12-06 | 2011-05-04 | 东华大学 | Preparation method of narrow-distribution cellulose nanocrystalline |
| CN102532589A (en) * | 2011-12-21 | 2012-07-04 | 北京泰合源通生物科技有限公司 | Comprehensive recycling method of waste and old compact discs |
| CN103382225A (en) * | 2013-07-22 | 2013-11-06 | 浙江理工大学 | Surface esterification modification method for cellulose nanocrystalline |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040663A (en) * | 2010-12-06 | 2011-05-04 | 东华大学 | Preparation method of narrow-distribution cellulose nanocrystalline |
| CN102532589A (en) * | 2011-12-21 | 2012-07-04 | 北京泰合源通生物科技有限公司 | Comprehensive recycling method of waste and old compact discs |
| CN103382225A (en) * | 2013-07-22 | 2013-11-06 | 浙江理工大学 | Surface esterification modification method for cellulose nanocrystalline |
Non-Patent Citations (1)
| Title |
|---|
| Weinan Xu et al.Cellulose nanocrystals as organic nanofillers for transparent polycarbonate films.《J Nanopart Res》.2013,第15卷(第4期),1-8. * |
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