CN106317578A - High-ultraviolet-shielding high-barrier nanomaterial film and preparation method thereof - Google Patents
High-ultraviolet-shielding high-barrier nanomaterial film and preparation method thereof Download PDFInfo
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
Abstract
The invention belongs to the field of preparation of polymer materials and discloses a high-ultraviolet-shielding high-barrier nanomaterial film and a preparation method thereof; ethanolamine functionalized graphene nanoribbons are dispersed in low-density polyethylene base to produce masterbatch; the masterbatch is mixed with low-density polyethylene granules according to a mass ratio of 1:1 and is extruded, pelletized and sheeted and cut into the nanomaterial film; in the nanomaterial film, the ethanolamine functionalized graphene nanoribbons account for 0.2-1.5% by weight of the low-density polyethylene base; the graphene oxide nanoribbons herein are subjected to ethanolamine modification, the ability of the nanoribbons to dissolve in an organic solvent is improved, and the nanoribbons can be dispersed evenly in LDPE (low-density polyethylene) base; by tightly combining ethanolamine functionalized graphene nanoribbon intercalation with the LDPE base, the composite material is provided with excellent barrier property; by introducing ethanolamine, the ultraviolet shielding property of the composite film is greatly improved; the film is applicable to the field of ultraviolet shielding and barrier packaging film and has a promising application prospect.
Description
Technical field
The invention belongs to field of polymer material preparing technology, be specifically related to a kind of high ultraviolet shielded high barrier nanometer material
Material thin film and preparation method thereof.
Background technology
Polyethylene (PE) is the aggregated prepared a kind of thermoplastic resin of ethylene, and simple in construction, is also most widely used high score
Sub-material.The nontoxic odorless of polyethylene, has excellent high extensibility, resistance to low temperature, and chemical stability is good, is resistant to most of acid
The erosion of alkali；Being widely used in industry, agricultural, packaging and daily industry, in China, application is the most extensive.But polyethylene
Thin film is disadvantageous in that, little molecule such as oxygen, steam etc. are readily permeable goes out for some, and ultraviolet is easily perforated through simultaneously
Go, significantly limit the application in terms of ultraviolet screener, obstruct of the PE thin-film material.So improving the performance of PE further,
Its functionalization is made to become the emphasis of research.
In order to improve ultraviolet screener performance and the barrier property of thin-film material, it may be considered that uniformly divide in TPU matrix
Dissipate the appropriate filler with high performance efficiency, so that thin film reaches the effect of anticipation.Graphene nanobelt (GNRs) is one
Plant the thin ribbon shaped structural material being mainly made up of carbon atom, can be regarded as a kind of special construction two-dimensional variation of Graphene.
GNRs is in addition to having the excellent physics of Graphene, chemistry and mechanical performance, due to the draw ratio that self is higher, little to water etc.
Molecular substance is stable, high-specific surface area, low defect, form is adjustable, thus has the raising polymer resistance more excellent than Graphene
Every ability, be with a wide range of applications.
Ethanolamine functionalized graphene nano belt is scattered in LDPE resin matrix by the present invention, in double screw extruder
Melting extruding pelletization, finally utilizes vulcanizing press to prepare EGNRs/LDPE composite material film, to its property through tabletting cutting
Can study, the introducing of ethanolamine greatly strengthen the uv-shielding capacity of composite material film and graphene nanobelt at base
Dispersibility in body；The EGNRs/ LDPE composite material film prepared is made to have the ultraviolet shielded and barrier property of excellence, from
And make the present invention have innovative value academicly, there is social benefit in actual applications widely.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of high ultraviolet shielded high barrier nano material
Thin film and preparation method thereof.The present invention is by combining closely so that composite material film has between EGNRs intercalation and LDPE matrix
There are uv-shielding capacity and the barrier property of excellence.
For realizing the purpose of the present invention, adopt the following technical scheme that
The preparation method of a kind of high ultraviolet shielded high barrier nano material film: by ethanolamine functionalized graphene nano belt
(EGNRs) it is scattered in low-density polyethylene body and prepares masterbatch；Masterbatch is mixed by 1:1 mass ratio with Low Density Polyethylene pellet
After, extruded pelletize, tabletting cutting prepare nano material film；In described nano material film, ethanolamine-functionalized graphite
It is 0.2% ~ 1.5% that alkene nano belt accounts for the mass content of low-density polyethylene body.
The preparation method of described ethanolamine functionalized graphene nano belt is: by stannic oxide/graphene nano band (GONRs)
With ethanolamine after 25 DEG C of reaction 24h, lyophilization prepares modified graphene oxide nano belt (EGONRs)；By modified oxidized stone
Ink alkene nano belt is dispersed in deionized water, adds hydrazine hydrate, 100 DEG C of reaction 6 h, prepares ethanolamine functionalized graphene
Nano belt (EGNRs).
The melt index values of described low-density polyethylene body be 1.0 ~ 3.0 g/10 min, preferably scope be 1.5 ~
2.0g/10min。
The preparation method of described height ultraviolet shielded high barrier nano material film: ethanolamine functionalized graphene is received
Rice band is scattered in dimethylbenzene, is ultrasonically formed homodisperse nanometer solution；It is subsequently adding Low Density Polyethylene, and is warming up to 80
DEG C, stirring is to liquid/paste；Then liquid/paste is poured into stirring flocculation in dehydrated alcohol, filters and be dried, obtain masterbatch；With
After masterbatch and Low Density Polyethylene pellet 1:1 in mass ratio added in double screw extruder melt extrude pelletize, finally utilize
Vulcanizing press prepares nano material film through tabletting cutting；In nanometer solution, ethanolamine functionalized graphene nano belt is dense
Degree is 0.002 mg mL-1；Described melt temperature is 140 DEG C.
The height ultraviolet shielded high barrier nano material film that a kind of preparation method as above prepares.
The functionalized nano material film material prepared through the inventive method has the uv-shielding capacity of excellence, barrier
Can, can apply in actual production in terms of ultraviolet release workshop, sunshade equipment and in terms of packaging, there is wide reality
Using value.
The beneficial effects of the present invention is:
1) the ethanolamine functionalized graphene nano belt through hydrazine hydrate reduction gained has the draw ratio of excellence, low defect, knot
The features such as structure is fine and close, on the one hand owing to introducing ethanolamine, improve the lipophile of graphene nanobelt, it is achieved that it is at diformazan
In benzene dispersed, good with low-density polyethylene compatability, provide the foundation for preparing composite material film；On the other hand
The introducing of ethanolamine, the character unique due to ethanolaminated graphene nanobelt and being uniformly distributed in the base, for excellent
Ultraviolet shielded and barrier property provides the foundation, and greatly strengthen the uv-shielding capacity of composite nano materials thin film；
2) preparation method of the present invention is scientific and reasonable, operation simple, strong operability, prepares LDPE composite nano materials thin film safety collar
Protect, there is the uv-shielding capacity of excellence, barrier property；Can apply in actual production simultaneously ultraviolet discharge workshop,
Sunshade equipment aspect and packaging aspect, improve value-added content of product, greatly extends the range of application of ldpe film, has
Market prospect and significant economic results in society widely.
Accompanying drawing explanation
Figure 1A is (a) GONRs, the FTIR of (b) EGONRs and (c) EGNRs spectrum；
Figure 1B is that (solution concentration is 0.5 mg to (1) GONRs, (2) EGONRs and (3) EGNRs scatter diagram in dimethylbenzene
mL-1, after standing 15d)；
Fig. 2 is the scanning electron microscope analysis figure (SEM) after the section metal spraying of quenching of EGNRs/LDPE nano material film sample；
The OTR oxygen transmission rate change song of LDPE nano material film when Fig. 3 is pure ldpe film and interpolation difference Nano filling
Line；
The ultraviolet ray transmissivity curve of LDPE nano material film when Fig. 4 is pure ldpe film and interpolation difference Nano filling.
Detailed description of the invention
For the openest rather than restriction present invention, below in conjunction with example, the present invention is described in further detail.
A kind of method of high ultraviolet shielded high barrier nano material film, concretely comprises the following steps:
(1) preparation of GONRs: first by the 180 dense H of mL2SO4It is slowly added in round-bottomed flask stirring, then by 20 mL
H3PO4Slowly instill, mix homogeneously under certain rotating speed, 1 g MWCNTs is slowly added to and stirs 30 min to uniformly, then will
6 g KMnO4It is slowly added in liquid mixed above；Drop after above-mentioned reaction system is stirred in the oil bath of 50 DEG C reaction 24 h
Warm to room temperature, be then poured into containing 10 mL H2O2500 mL deionized waters in ice bath stir 1 h, now solution becomes ink
Green explanation reaction fully, is subsequently adding appropriate HCl and is centrifuged to neutrality, be finally dried to obtain GONRs in freezer dryer；
(2) preparation of EGONRs: be dissolved in 100 mL deionized waters by 100 mg GONRs, ultrasonic 1 H-shaped of 100W uniformly divides
Dissipate liquid；Add certain HCl, regulate pH to 1 ~ 2；Being subsequently adding 0.5 g ethanolamine room temperature reaction 24 h, the black paste obtained produces
Thing, with dehydrated alcohol and deionized water wash repeatedly to remove remaining ethanolamine and HCl, is finally dried in freezer dryer
Obtain EGONRs；
(3) preparation of EGNRs: 100 mg EGONRs are dissolved in 100 mL deionized waters, ultrasonic 1 H-shaped of 100W uniformly disperses
Liquid, adds 1 g hydrazine hydrate, reduces 6 h at 100 DEG C；The black paste product obtained, with dehydrated alcohol and deionized water wash
Repeatedly to remove remaining hydrazine hydrate, in freezer dryer, finally it is dried to obtain EGNRs；
(4) preparation of EGNRs/LDPE laminated film: take 5 g LDPE and be placed in round-bottomed flask, adds 30 mL dimethylbenzene, rises
Temperature is to 80 DEG C and stirs to liquid/paste, is dissolved in 10mL dimethylbenzene by 0.05 g EGNRs, is then poured slowly into round-bottomed flask
In, and stir under certain rotating speed；Mixed liquor is poured into slowly stirring flocculation in substantial amounts of dehydrated alcohol, filters and do
Dry, obtain EGNRs/LDPE masterbatch；Subsequently gained EGNRs/LDPE masterbatch and LDPE pellet are pressed 1:1 and add double screw extruder
In at 140 DEG C melting extruding pelletization, to prepare thickness be that 0.5 mm difference contains through tabletting cutting finally to utilize vulcanizing press
The EGNRs/LDPE composite material film of amount.
Comparative example 1
Take 5 g LDPE to be placed in round-bottomed flask, add 30 mL dimethylbenzene, be warming up to 80 DEG C and stir to liquid/paste, will stick with paste
Shape liquid pours stirring flocculation in substantial amounts of dehydrated alcohol lentamente into, filters and is dried, obtains LDPE masterbatch；Subsequently by gained
LDPE masterbatch and LDPE pellet add in double screw extruder melting extruding pelletization at 140 DEG C by 1:1 ratio, finally utilize and put down
It is 0.5 mm ldpe film that plate vulcanizer prepares thickness through tabletting cutting.
Embodiment 1
Take 5 g LDPE to be placed in round-bottomed flask, add 30 mL dimethylbenzene, be warming up to 80 DEG C and stir to pasty state；By 0.05 g
EGNRs is dissolved in 10mL dimethylbenzene, is poured slowly in round-bottomed flask, and stirs；Mixed liquor is poured into slowly substantial amounts of
In dehydrated alcohol, stirring flocculation, filters and is dried, and obtains EGNRs/LDPE masterbatch, subsequently by gained EGNRs/LDPE masterbatch with
LDPE pellet is pressed 1:1 and is added in double screw extruder melting extruding pelletization at 140 DEG C, finally utilizes vulcanizing press through tabletting
0.5wt%EGNRs/LDPE composite material film is prepared in cutting.
Embodiment 2
Take 12.5 g LDPE to be placed in round-bottomed flask, add 60 mL dimethylbenzene, be warming up to 80 DEG C and stir to pasty state；By 0.05
G EGNRs is dissolved in 10mL dimethylbenzene, is poured slowly in round-bottomed flask, and stirs；Mixed liquor is poured into slowly a large amount of
Dehydrated alcohol in stirring flocculation, filter and be dried, obtain EGNRs/LDPE masterbatch, subsequently by gained EGNRs/LDPE masterbatch with
LDPE pellet is pressed 1:1 and is added in double screw extruder melting extruding pelletization at 140 DEG C, finally utilizes vulcanizing press through tabletting
0.2wt%EGNRs/LDPE composite material film is prepared in cutting.
Embodiment 3
Take 6.25 g LDPE to be placed in round-bottomed flask, add 40 mL dimethylbenzene, be warming up to 80 DEG C and stir to pasty state；By 0.05
G EGNRs is dissolved in 10mL dimethylbenzene, is poured slowly in round-bottomed flask, and stirs；Mixed liquor is poured into slowly a large amount of
Dehydrated alcohol in stirring flocculation, filter and be dried, obtain EGNRs/LDPE masterbatch；Subsequently by gained EGNRs/LDPE masterbatch with
LDPE pellet is pressed 1:1 and is added in double screw extruder melting extruding pelletization at 140 DEG C, finally utilizes vulcanizing press through tabletting
0.4wt%EGNRs/LDPE composite material film is prepared in cutting.
Embodiment 4
Take 4.17 g LDPE to be placed in round-bottomed flask, add 30 mL dimethylbenzene, be warming up to 80 DEG C and stir to pasty state；By 0.05
G EGNRs is dissolved in 10mL dimethylbenzene, is poured slowly in round-bottomed flask, and stirs；Mixed liquor is poured into slowly a large amount of
Dehydrated alcohol in stirring flocculation, filter and be dried, obtain EGNRs/LDPE masterbatch；Subsequently by gained EGNRs/LDPE masterbatch with
LDPE pellet is pressed 1:1 and is added in double screw extruder melting extruding pelletization at 140 DEG C, finally utilizes vulcanizing press through tabletting
0.6wt%EGNRs/LDPE composite material film is prepared in cutting.
Embodiment 5
Take 3.125 g LDPE to be placed in round-bottomed flask, add 30 mL dimethylbenzene, be warming up to 80 DEG C and stir to pasty state；Will
0.05 g EGNRs is dissolved in 10mL dimethylbenzene, is poured slowly in round-bottomed flask, and stirs；Mixed liquor is poured into slowly
In substantial amounts of dehydrated alcohol, stirring flocculation, filters and is dried, obtain EGNRs/LDPE masterbatch；Subsequently that gained EGNRs/LDPE is female
Material with LDPE pellet press 1:1 addition double screw extruder at 140 DEG C melting extruding pelletization, finally utilize vulcanizing press warp
0.8wt%EGNRs/LDPE composite material film is prepared in tabletting cutting.
Embodiment 6
Take 2.5 g LDPE to be placed in round-bottomed flask, add 30 mL dimethylbenzene, be warming up to 80 DEG C and stir to pasty state；By 0.05
G EGNRs is dissolved in 10mL dimethylbenzene, is poured slowly in round-bottomed flask, and stirs；Mixed liquor is poured into slowly a large amount of
Dehydrated alcohol in stirring flocculation, filter and be dried, obtain EGNRs/LDPE masterbatch；Subsequently by gained EGNRs/LDPE masterbatch with
LDPE pellet is pressed 1:1 and is added in double screw extruder melting extruding pelletization at 140 DEG C, finally utilizes vulcanizing press through tabletting
1.0wt%EGNRs/LDPE composite material film is prepared in cutting.
Embodiment 7
Take 1.7 g LDPE to be placed in round-bottomed flask, add 30 mL dimethylbenzene, be warming up to 80 DEG C and stir to pasty state；By 0.05
G EGNRs is dissolved in 10mL dimethylbenzene, is poured slowly in round-bottomed flask, and stirs；Mixed liquor is poured into slowly a large amount of
Dehydrated alcohol in stirring flocculation, filter and be dried, obtain EGNRs/LDPE masterbatch；Subsequently by gained EGNRs/LDPE masterbatch with
LDPE pellet is pressed 1:1 and is added in double screw extruder melting extruding pelletization at 140 DEG C, finally utilizes vulcanizing press through tabletting
1.5wt%EGNRs/LDPE composite material film is prepared in cutting.
Claims (7)
1. the preparation method of one kind high ultraviolet shielded high barrier nano material film, it is characterised in that: by ethanolamine-functionalized
Graphene nanobelt is scattered in low-density polyethylene body and prepares masterbatch；1:1 mass pressed by masterbatch and Low Density Polyethylene pellet
After mixing, extruded pelletize, tabletting cutting prepare nano material film；In described nano material film, ethanolamine function
It is 0.2% ~ 1.5% that functionalized graphene nano belt accounts for the mass content of low-density polyethylene body.
The preparation method of height the most according to claim 1 ultraviolet shielded high barrier nano material film, it is characterised in that:
The preparation method of described ethanolamine functionalized graphene nano belt is: by anti-at 25 DEG C to stannic oxide/graphene nano band and ethanolamine
After answering 24h, lyophilization prepares modified graphene oxide nano belt；Modified graphene oxide nano belt is dispersed in from
In sub-water, add hydrazine hydrate, 100 DEG C of reaction 6 h, prepare ethanolamine functionalized graphene nano belt.
The preparation method of height the most according to claim 1 ultraviolet shielded high barrier nano material film, it is characterised in that:
The melt index values of described low-density polyethylene body is 1.0 ~ 3.0 g/10 min.
The preparation method of height the most according to claim 1 ultraviolet shielded high barrier nano material film, it is characterised in that:
Ethanolamine functionalized graphene nano belt is scattered in dimethylbenzene, is ultrasonically formed homodisperse nanometer solution；It is subsequently adding
Low Density Polyethylene, and it is warming up to 80 DEG C, stirring is to liquid/paste；Then liquid/paste is poured into stirring wadding in dehydrated alcohol
Solidifying, filter and be dried, obtain masterbatch；Subsequently masterbatch is added twin-screw extrusion with Low Density Polyethylene pellet 1:1 in mass ratio
Machine melt extrudes pelletize, finally utilizes vulcanizing press to prepare nano material film through tabletting cutting.
The preparation method of height the most according to claim 1 ultraviolet shielded high barrier nano material film, it is characterised in that:
In nanometer solution, the concentration of ethanolamine functionalized graphene nano belt is 0.002 mg mL-1。
The preparation method of height the most according to claim 1 ultraviolet shielded high barrier nano material film, it is characterised in that:
Described melt temperature is 140 DEG C.
7. the height ultraviolet shielded high barrier nano material that the preparation method as described in any one of claim 1-6 prepares is thin
Film.
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| CN201610815042.XA CN106317578A (en) | 2016-09-12 | 2016-09-12 | High-ultraviolet-shielding high-barrier nanomaterial film and preparation method thereof |
| PCT/CN2016/111410 WO2018045671A1 (en) | 2016-09-12 | 2016-12-22 | Nanomaterial film with high ultraviolet shielding and high barrier properties and preparation method therefor |
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| WO2018045671A1 (en) * | 2016-09-12 | 2018-03-15 | 福州大学 | Nanomaterial film with high ultraviolet shielding and high barrier properties and preparation method therefor |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2018045671A1 (en) * | 2016-09-12 | 2018-03-15 | 福州大学 | Nanomaterial film with high ultraviolet shielding and high barrier properties and preparation method therefor |
| CN107141562A (en) * | 2017-06-19 | 2017-09-08 | 南通强生光电科技有限公司 | Uvioresistant anti-aging modified graphene oxide electric wire and cable material and preparation and application |
| CN107715702A (en) * | 2017-11-14 | 2018-02-23 | 天津工业大学 | A kind of gas-liquid membrane contactor alkamine modified graphene oxide/polyvinylidene fluoride blending film and preparation method thereof |
| CN110055031A (en) * | 2019-05-28 | 2019-07-26 | 安徽科技学院 | A kind of preparation method of width ultravioletvisible absorption Graphene composite thin film material |
| CN110055031B (en) * | 2019-05-28 | 2022-04-01 | 安徽科技学院 | Preparation method of wide ultraviolet visible absorption graphene composite film material |
| CN113979428A (en) * | 2021-11-17 | 2022-01-28 | 深圳市鸿富诚屏蔽材料有限公司 | Preparation method of heat-conducting wave-absorbing composite film and heat-conducting wave-absorbing composite film |
| CN114456470A (en) * | 2022-03-09 | 2022-05-10 | 中海石油(中国)有限公司 | Polymer composite material with gas high-barrier property |
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