CN103059434A - Method for preparing high-resistant polystyrene composite film - Google Patents
Method for preparing high-resistant polystyrene composite film Download PDFInfo
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- CN103059434A CN103059434A CN2013100092278A CN201310009227A CN103059434A CN 103059434 A CN103059434 A CN 103059434A CN 2013100092278 A CN2013100092278 A CN 2013100092278A CN 201310009227 A CN201310009227 A CN 201310009227A CN 103059434 A CN103059434 A CN 103059434A
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Abstract
The invention discloses a method for preparing a high-resistant polystyrene composite film. Graphene oxides (GONSs) are taken as an efficient lamellar nanometer barrier reinforcing filler and wraps a polystyrene (PS) surface in a solution mixing and reduced pressure distillating manner, so that a GONSs/PS micro barrier unit is obtained and assembled to a GONSs/PS composite film with a barrier structure. According to the prepared nano-composite film, GONSs are distributed on a PS particle boundary to form a unique barrier structure; gas can permeate along a tortuous path in a composite film permeation process with the combination of the successfully built micro structure and good GONSs gas barrier performance, and thus, the composite film with high barrier performance is obtained; and moreover, the method adopts a solution mixing and hot-press forming processing mode, is simple in preparation method, easy in technology mastering and low in production cost, and has great large-scale production potential.
Description
Technical field
The invention belongs to polymer packaging film field, relate to the preparation method of a kind of high-barrier graphene oxide (hereinafter to be referred as GONSs)/polystyrene (hereinafter to be referred as PS) laminated film.
Background technology
Compare with traditional wrapping material such as glass, metal and pottery etc., polymeric film such as polyethylene (PE), polypropylene (PP), polystyrene (PS) and polyester (PET) etc. are with the mechanical property of excellence, outstanding moulding processability, good weathering resistance, the transparency and chemical stability and cheap price, (Kenneth Marsh has a wide range of applications in food and drug packaging field, et al.Journal ofFood and Science, 2007,72:39-55).But single polymeric film is limited to the barrier property of gas, is difficult to satisfy the service requirements of different commodity.Therefore, in order to prolong the shelf-life of commodity, guarantee that commodity never degenerate when storing, transport, processing and distributing, protect fragrant guarantor and distinguish the flavor of, prepare " focus " problem that the polymer thin-film material with high obstructing performance becomes contemporary packaging industry and plastics industry.
At present, the method that improves the polymeric film barrier property mainly contains vacuum evaporation (Semyra Vasquez-Borucki, et al.Diamond and Related Materials, 2000,9:1971-1978.), multi-layer co-extruded compound, the compound (O.Urresti of laminar nano filler, et al.Journal ofMembrane Science, 2011,373:173-177.).Wherein, the barrier coat that adopts vacuum evaporation technology to obtain is very thin, easily crack when being subject to external impacts, and the layering that comes off, thus affect its barrier property; Each layer thickness mainly relies on the forcing machine speed adjustment in the film of multi-layer co-extruded compounding technology preparation, and this is higher to processing peopleware and processing units dependency; The laminar nano filler is compound to be that a small amount of nanoscale twins filler (such as nanoclay) is filled in the polymeric matrix, utilize the good interface interaction of polymkeric substance and Nano filling and nanoscale twins filler in polymeric matrix, to cause " multipath effect " or " nanometer barrier wall effect " of gas-permeable, effectively improve the barrier property of polymeric matrix.It is high and be beneficial to the advantage such as recovery that laminar nano filler compounding technology has easy, the product cost performance of processing, and be conducive to wrapping material to high performance, functionalization future development, is considered to the technology that modern plastics Barrier Technology field has future.Improve the nanoscale twins filler of nano composite material barrier property normally take nanoclay as main, but, research find the dispersing morphology of nanoclay in polymeric matrix mainly take reunite and intercalation as main, this is totally unfavorable to the barrier property that improves matrix material, has also limited the widespread use of polymer composite film at packaging field.Therefore, prepare high-barrier nano composite material, must seek a kind of high-barrier nano lamella filler and make up the polymkeric substance condensed state structure with excellent barrier properties, this also is the study hotspot for preparing at present high-barrier composite material.In novel high-barrier nano stratified material, Graphene (GNSs) is with machinery, calorifics, electricity and the barrier property of its excellence, field of new have huge application potential (Novoselov K S, et al.Science, 2004,306:666-669).Graphene oxide (GONSs) is a kind of oxidized derivatives of GNSs, is the bi-dimensional cellular shape material that is closely linked by the monolayer carbon atom, has great specific surface area and geometric properties ratio.And have a large amount of oxygen-containing functional groups on the GONSs laminated structure, as carbonyl (C=O), carboxyl (COOH), hydroxyl (OH) and epoxy group(ing) (C-O-C) (He H, et al.Chemical Physics Letter, 1998,287:53-56.).These groups provide a large amount of reactive behavior points, not only can form good interface interaction with matrix, and can realize that GONSs fully peels off and Uniform Dispersion in matrix.Therefore, GONSs is a kind of efficient nano lamella filler for preparing high-barrier nano composite material.
Except selecting high barrier material, from the angle of polymer processing, by microscopic pattern and the dispersion state of lamella Nano filling in polymeric matrix of processing outfield regulation and control polymer composite material, also can improve the barrier property of matrix material.Wherein, the layer-by-layer structure be exactly " sandwich " structure of alternately assembling by polymeric matrix and nanoscale twins filler (MorganAPriolo, et al.Nano Letter, 2010,10:4970-4974.).The advantage of this structure maximum is that the nanoscale twins filler in polymeric matrix camber orientation, directional profile, has greatly improved the zigzag path of gas-permeable, thereby obtains the nano composite material that superelevation intercepts.In addition, we research during conductive nano composite material (Pang H, et al.Materials Letters, 2010,64:2226-2229.), obtained a kind of isolation structure system that has characteristic.Its principle is that full-bodied ultrahigh molecular weight polyethylene(UHMWPE) (UHMWPE) matrix can stop the GNSs filler to enter polymer particle inside effectively, makes it be distributed in the UHMWPE particle surface.This structure not only has larger application prospect in the conduction field, and simultaneously, its Nano filling also provides strong evidence for its application in the field of obstruct in the special distribution form of polymer beads sub-surface.
Based on above research work, we are by the complete air-locked high obstructing performance of GONSs, the method that adopts solution to mix is wrapped in the PS particle surface with it, then utilize hot-press forming device, make up the GONSs/PS recombiner unit of high-barrier, formation has the nano compound film of isolation structure, thereby preparation has the high-barrier GONSs/PS nano composite material of isolation structure.Compare with traditional high-barrier nano composite material, the barrier property of related nano composite material is along with there is " obstruct exceed an ooze " phenomenon in the increase of GONSs content among the present invention, be that GONSs content is when low, the barrier property of compound system improves not obvious, but when GONSs reached a threshold value, the barrier property of compound system increased significantly.
From looking into patent, at present about utilizing Graphene to prepare the patent of high-barrier composite material and few, and the patent of utilizing isolation structure to prepare Graphene/polystyrene high-barrier nano composite material has no report especially.
Summary of the invention
Characteristics for single polymers thin-film barrier poor performance, to improve the polymeric film barrier property as purpose, the present invention proposes to intercept reinforcing filler with GONSs as efficient laminar nano, be coated on the polymer particles surface by solution mixing, underpressure distillation, at hot-forming middle unique isolation structure that makes up, thereby improve polymer composite film to the barrier property of oxygen, a kind of preparation method with high-barrier nano laminated film of isolation structure is provided.
A kind of preparation method with high-barrier nano laminated film of isolation structure provided by the invention comprises following processing step:
(1) graphene oxide suspension preparation: graphite oxide is joined in the ethanolic soln, and ultrasonic agitation realizes that graphite oxide effectively peels off Uniform Dispersion in ethanolic soln, prepares the alcohol suspension of GONSs;
(2) solution mixes: the PS powder is joined in the GONSs alcohol suspension that step (1) obtains, and is 98 ~ 99.5:0.5 ~ 2 by PS powder and GONSs weight ratio; Underpressure distillation under ultrasonic agitation, suction filtration is removed ethanolic soln, and leftover materials are drying treatment in the convection oven of 60 ° of C, until the content of solvent is lower than 0.01%, thereby obtains the PS composite particles that GONSs coats;
(3) hot-forming: PS composite particles preheating under 180 ~ 200 ° of C that the GONSs that step (2) is obtained coats is not less than 5min, then to be not less than under the 10MPa more than the hot pressing 5min, to be cooled to room temperature under the 10MPa and to obtain target product being not less than at last.
More than the equal percentage ratio meter by weight of umber of used graphene oxide and PS powder.
The inventive method is to adopt to have the GONSs of unique two-dimentional laminated structure as the barrier property toughener, by little blocker unit that solution mixes, underpressure distillation prepares GONSs coating PS particle, recycle hot-forming mode, the little blocker unit of PS that GONSs is coated bonds together, and makes up the nano compound film with isolation structure.The GONSs/PS laminated film that obtains is compared with pure PS film, has the gas barrier property of superelevation, and its oxygen permeability coefficient is 1.226 * 10
-16Cm
3Cm/cm
2SPa has reduced about 99.91%.In addition, advantage of the present invention also is embodied in the following aspects:
(1) the present invention adopts GONSs as the barrier property toughener, and its unique two-dimensional nano laminated structure is given its remarkable gas barrier property, and the raw material sources of preparation GONSs are extensive, cheap;
(2) the present invention is coated on the PS microparticle surfaces with GONSs, makes up little blocker unit, with this micro unit in hot-forming, mutually bonding prepares the nano compound film with isolation structure.The GONSs lamella filler of high-barrier and special isolation structure are organically combined, proposed a kind of preparation method of high-barrier nano composite material of novelty.
(3) the present invention adopts that solution mixes, hot-forming processing mode, and the preparation method is simple, and technique is easy to grasp, and production cost is low, and the potentiality of scale operation are arranged.
Description of drawings is as follows:
Fig. 1 is the preparation synoptic diagram of GONSs/PS nano compound film;
Fig. 2 is that graphene oxide is dispersed in the atomic force microscope figure in the ethanolic soln;
Fig. 3 is the scanning electron microscope diagram that GONSs is coated on the PS microparticle surfaces;
Fig. 4 is the opticmicroscope figure of GONSs/PS laminated film cross section;
Embodiment
Embodiment given below is to specific descriptions of the present invention; be necessary to be pointed out that at this following examples are only for the present invention is further illustrated; can not be interpreted as limiting the scope of the invention, this art skilled person still belongs to protection scope of the present invention according to the invention described above content to nonessential improvement and the adjustment that the present invention makes.Preparation technology's flow process of sample of the present invention as shown in Figure 1, wherein the PS particulate can be with directly synthetic or the way that pellet carries out mechanical disintegration obtained, its particle diameter is about 20 ~ 80 μ m.
Graphite oxide in following examples is the laboratory preparation, the raw material that adopts is expanded graphite, method is improved Hummers method: first expanded graphite is joined concentration and be in 98% the vitriol oil, mix, add the 1g expanded graphite in per 23 ~ 50ml vitriol oil; Subsequently, under the effect of stirring, in above-mentioned mixing solutions, add KMnO lentamente
4, KMnO
4Weight be 3 ~ 7 times of expanded graphite, the temperature of the hierarchy of control is at 35 ~ 40 ° of C, stirs that slowly to add with the expanded graphite weight ratio behind the 1h be the deionized water of 1:20 ~ 1:50, adds will prevent in the water process because diluting dense H
2SO
4System temperature surpasses 100 ° of C, then leaves standstill 0.5 ~ 2h, and using with the expanded graphite weight ratio is the deionized water dilution of 1:120 ~ 1:250, and adds the H of 1 ~ 3 times of expanded graphite weight
2O
2(concentration 30%), this moment, mixed solution can produce bubbling and intensification, was jonquilleous suspension by brown stain.Filtering suspension liquid is also used the HCl solution repetitive scrubbing of 1:10, to remove metal ion and SO
4 2-Use again a large amount of deionized water repetitive scrubbings, until pH value is near 7, then utilize ultrasonic wave to be scattered in the deionized water mashed prod on the filter paper, centrifugal 20 ~ 80min is to remove the graphite oxide of not peeling off under the rotating speed of 2000 ~ 8000rpm, at last dispersion liquid is dehydrated under 60 ~ 80 ° of C, until the weight content of moisture prepares graphite oxide less than 0.01%.
The weight-average molecular weight of used PS is 18 ~ 350,000.
Embodiment 1 ~ 8
(1) preparation graphene oxide suspension: a certain amount of graphite oxide and 400ml ethanolic soln are joined in the there-necked flask, concrete prescription such as table 1, then ultrasonic and stir 3h, realize graphite oxide effectively peeling off in ethanolic soln, Uniform Dispersion, prepare the alcohol suspension of GONSs.
(2) solution mixes: a certain amount of PS particulate is joined in the GONSs alcohol suspension that obtains in the step (1), concrete prescription such as table 1, then under the acting in conjunction of ultrasonic and stirring, adopt the mode of underpressure distillation, suction filtration is removed most ethanolic soln, remaining solution is drying treatment in the convection oven of 60 ° of C, until the weight content of solvent is lower than 0.01%, thereby obtains the PS composite particles that GONSs coats.
(3) hot-forming: PS composite particles preheating 5min under 180 ~ 200 ° of C that the GONSs that step (2) is obtained coats, concrete hot-forming temperature sees Table 1, then with hot pressing 5min under the 10MPa, is cooled at last room temperature and obtains target product under 10MPa.
Comparative Examples 1 ~ 2
(1) Comparative Examples 1, and each weight percentages of components by Comparative Examples in the table 11 provides with material preheating 5min under 180 ° of C, then with hot pressing 5min under the 10MPa, is cooled at last room temperature and obtains pure PS sample for Performance Ratio under 10MPa.
(2) Comparative Examples 2, each weight percentages of components that provides by Comparative Examples in the table 12, with the processing step of material according to embodiment 1 ~ 8, preheating 5min under 180 ° of C then, then with hot pressing 5min under the 10MPa, under 10MPa, be cooled at last room temperature and obtain target product.
The prescription of table 1 embodiment 1 ~ 7 and Comparative Examples 1 ~ 2 and hot-forming temperature
| Embodiment | GONSs/ weight fraction (%) | PS particulate/weight fraction (%) | Hot-forming temperature (° C) |
| 1 | 0.5 | 99.5 | 180 |
| 2 | 0.5 | 99.5 | 190 |
| 3 | 0.5 | 99.5 | 200 |
| 4 | 1 | 99 | 180 |
| 5 | 1 | 99 | 190 |
| 6 | 1 | 99 | 200 |
| 7 | 2 | 98 | 190 |
| 8 | 2 | 98 | 200 |
| Comparative Examples 1 | 0 | 100 | 180 |
| Comparative Examples 2 | 2 | 98 | 180 |
In order to investigate extent of exfoliation and the dispersion state of GONSs in ethanolic soln, the present invention has adopted atomic force microscope that the lamellar spacing of GONSs has been carried out detecting (Fig. 2), find the about 1nm of lamellar spacing of GONSs, show that GONSs has obtained peeling off fully, obtained uniform and stable GONSs alcohol suspension; In order to estimate feasibility and form and the distribution of GONSs in PS microparticle surfaces and laminated film of this isolation structure high-barrier nano composite material of preparation, scanning electronic microscope (Fig. 3) has characterized the coating situation of GONSs at the PS microparticle surfaces, find the surface that is coated on the PS particulate of GONSs success, and show the typical pattern of fold, the π-πconjugation that this is mainly derived between GONSs and the PS has formed the absorption coating of GONSs to the PS microparticle surfaces; Adopt opticmicroscope (Fig. 4) to observe the little blocker unit of GONSs/PS in hot pressing, the bonding of little blocker unit and the formational situation of isolation structure.As can be seen from Figure 4, larger distortion has occured in the PS particulate in hot pressing, but GONSs still is distributed in the interface of different PS particulates, has formed unique isolation structure.The successful structure of this microstructure is added the good gas barrier property of GONSs, will cause gas in the laminated film process of osmosis, directly permeates along winding raod more, thereby obtains the laminated film (table 2) of excellent barrier property.
Table 2 embodiment and comparative example's oxygen barrier property synopsis
Claims (3)
1. the preparation method of a high-barrier polystyrene laminated film, intercept reinforcing filler with GONSs as efficient laminar nano, be coated on the polymer particles surface by solution mixing, underpressure distillation, at hot-forming middle unique isolation structure that makes up, thereby improve polymer composite film to the barrier property of oxygen, comprise the steps:
(1) graphene oxide suspension preparation: graphite oxide is joined in the ethanolic soln, and ultrasonic agitation realizes that graphite oxide effectively peels off Uniform Dispersion in ethanolic soln, prepares the alcohol suspension of GONSs;
(2) solution mixes: the PS powder is joined in the GONSs alcohol suspension that step (1) obtains, and is 98 ~ 99.5:0.5 ~ 2 by PS powder and GONSs weight ratio; Underpressure distillation under ultrasonic agitation, suction filtration is removed ethanolic soln, and leftover materials are drying treatment in the convection oven of 60 ° of C, until the content of solvent is lower than 0.01%, thereby obtains the PS composite particles that GONSs coats;
(3) hot-forming: PS composite particles preheating under 180 ~ 200 ° of C that the GONSs that step (2) is obtained coats is not less than 5min, then to be not less than under the 10MPa more than the hot pressing 5min, to be cooled to room temperature under the 10MPa and to obtain target product being not less than at last.
2. the preparation method of described high-barrier polystyrene laminated film according to claim 1 is characterized in that the weight-average molecular weight of described PS is 18 ~ 350,000.
3. method according to claim 1 is characterized in that, described graphite oxide adopts improvement Hummers legal system standby.
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| CN104015328A (en) * | 2014-05-27 | 2014-09-03 | 浙江金瑞薄膜材料有限公司 | Polyolefin high barrier film processing technology |
| CN104650498A (en) * | 2013-11-22 | 2015-05-27 | 中国科学院金属研究所 | Graphene/polymer composite conductive membrane material and preparation method thereof |
| CN106061593A (en) * | 2014-03-07 | 2016-10-26 | 汉阳大学校产学协力团 | Graphene oxide nanocomposite membrane having improved gas barrier characteristics and method for manufacturing same |
| CN107541033A (en) * | 2017-08-30 | 2018-01-05 | 华南理工大学 | A kind of high gas-obstructing character nano composite material and preparation method thereof |
| CN107629383A (en) * | 2017-09-08 | 2018-01-26 | 深圳市通产丽星股份有限公司 | A kind of graphene composite thin film material and preparation method thereof, application |
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| CN104650498A (en) * | 2013-11-22 | 2015-05-27 | 中国科学院金属研究所 | Graphene/polymer composite conductive membrane material and preparation method thereof |
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| CN110698826A (en) * | 2019-11-01 | 2020-01-17 | 四川大学 | Preparation method of high-barrier polylactic acid film containing three-dimensional barrier network |
| CN111303549A (en) * | 2020-04-07 | 2020-06-19 | 四川大学 | Preparation method of reinforced and toughened polystyrene and stretched film |
| CN111303549B (en) * | 2020-04-07 | 2021-10-08 | 四川大学 | Preparation method of reinforced and toughened polystyrene and stretched film |
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Application publication date: 20130424 |