CN109666208A - A kind of graphene oxide@SiO2The method of modified poly ethylene film - Google Patents
A kind of graphene oxide@SiO2The method of modified poly ethylene film Download PDFInfo
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- 239000004698 Polyethylene Substances 0.000 title claims abstract description 69
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 54
- -1 poly ethylene Polymers 0.000 title claims abstract description 21
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 14
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 14
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 14
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000003292 glue Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 90
- 239000000377 silicon dioxide Substances 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000741 silica gel Substances 0.000 claims description 9
- 229910002027 silica gel Inorganic materials 0.000 claims description 9
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 8
- 239000005457 ice water Substances 0.000 claims description 8
- 239000004115 Sodium Silicate Substances 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000010257 thawing Methods 0.000 claims description 6
- 238000005341 cation exchange Methods 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 239000012065 filter cake Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 239000000499 gel Substances 0.000 claims description 2
- 239000007800 oxidant agent Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 238000000108 ultra-filtration Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 229920002521 macromolecule Polymers 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 10
- 238000002834 transmittance Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002096 quantum dot Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- 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
- 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
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A kind of graphene oxide@SiO2The method of modified poly ethylene film belongs to macromolecule polymer material field.Blending and modifying solution is selected to carry out modified poly ethylene, selection modified material is graphene oxide@SiO2.The functional group of graphene oxide can prepare the solution of stable dispersion with PE association reaction, graphene oxide solution, therefore technological feasibility is good.Simultaneously because polyethylene can form a film and can pass through the modified molding that film may be implemented completely with the characteristic of glue.
Description
Technical field
The invention belongs to macromolecule polymer material field, in particular to a kind of graphene oxide@SiO2Modified poly ethylene
The preparation method of film.
Background technique
Polyethylene belongs to high molecular polymer, for making agricultural, food and industrial packaging film, wire and cable cladding
And coating, composed paper etc. are important industrial chemicals.Carbon aqueous polymer of the PE film as polyethylene, chemical component are determined
The environment compatibility of film and the recuperability of height are determined.And polyethylene film, it is slim and graceful transparent, there is moisture-proof, antioxygen, resistance to
Sour, the alkaline-resisting, performances such as air-tightness is general, and heat sealability is excellent.In order to make polyethylene preferably meet the market requirement, need thin to PE
Film is modified, to achieve the purpose that change or increase certain properties.The modification of PE can be divided into two kinds of methods: (1) being to PE
Coiled material is surface-treated, and forms polar group or polar monomer in its superficial layer；It (2) is first by highly polar PE graft
Or Macromolecular Surface Modifiers are mixed with PE, then manufacture coiled material with the methods of extrusion.
Graphene is a kind of single layer of carbon atom layer of 2D plane, and thickness only has 0.34nm, and the carbon between graphene is former
Son is closely connected, and the carbon atomic layer of plane, which can distort, under external force prevents from being broken, and thereby may be ensured that the steady of its structure
Determine, referred to as material most thin in universe.Graphene oxide (GO) is the important derivatives of graphene, and structure and graphene are substantially
Identical, difference is to be connected with the functional groups such as carboxyl, hydroxyl on the edge and face of carbon atomic layer.
Summary of the invention
PE modified to solve the problems, such as, the present invention provides a kind of graphene oxide SiO2Modified poly ethylene film
Preparation method, the preparation method comprise the steps of:
The preparation of step 1) silica gel solution
(1) sodium metasilicate is dissolved into sodium silicate aqueous solution, the sodium silicate aqueous solution is subjected to cation exchange removal Na
+, the silicate solution that mass fraction is 46% is obtained, wherein the partial size that cation exchanges resin used is 0.3-1.5mm, cation
It is stirred in exchange process using paddle, mixing speed is 180-200 revs/min；
(2) to the 10% amount silicate solution for step (1) is added at 85-92 DEG C into sodium hydroxide solution obtaining, heat preservation
0.8-1.2 hours obtained seed-solutions, seed-solution pH value are 9.0-9.7, wherein the weight ratio of silicate solution and sodium hydroxide
For 20:1；
(3) seed-solution in step (2) is taken, to the crystalline substance under the conditions of temperature is 85-92 DEG C, pH value is 9.0-9.7
The silicate solution of step (1) remaining 90% amount is added in kind, keeps the temperature 30-45 minutes after charging again, dilute silica gel must be synthesized；
(4) it is molten that the silica solution that silica quality percentage concentration is 40% is obtained after the dilute silica gel of synthesis being concentrated by ultrafiltration
Liquid；
Step 2) prepares graphene oxide modified solution
(1) graphene oxide is prepared
A. the concentrated sulfuric acid of 60ml is added in the reaction flask that 250mL is assembled in ice-water bath, then that 2.5g graphite powder is slow
It is added in the concentrated sulfuric acid, is persistently stirred in ice-water bath 1 hour；
B. 10g potassium permanganate and 3.8g sodium nitrate are slowly added by several times, stirring 2 hours is continued in ice-water bath；
C. remove ice-water bath, continue to stir 2 hours at normal temperature；
D. temperature is increased to 35 DEG C, continues stirring 2 hours；
E. temperature is controlled at 98 DEG C, is slowly added to deionized water, maintained water temperature to keep at 98 DEG C 1 hour, add simultaneously
Entering to treat percentage is that 30% hydrogen peroxide restores remaining oxidant, and mixture becomes glassy yellow from dark brown；
F. the mixture centrifuge separation obtained, and washed with 5%HCl solution and deionized water until sulfate radical-free in filtrate
Until being detected；
G. filter cake is placed in 60 DEG C of vacuum oven and is sufficiently dried, saved backup.
(2) graphene oxide prepared is added in the silica solution of step 1) preparation, obtains graphene oxide titanium dioxide
Silica sol modified solution；It is preferred that every 0.5-1.5g graphene oxide corresponds to silica solution 0.5-1ml；
Silica gel solution modified PE film forming is added in step 3) graphene oxide:
(1) gluey PE is taken to be added in reaction vessel, temperature is increased to 95 DEG C in water-bath, and stirring makes its thawing, directly
To when being stirred for, above choose no colloidal solid, the graphene oxide silicon dioxide gel that step 2) prepares is added at this time
Modified solution is stirred well to it and is uniformly dispersed, and water temperature in water-bath is dropped to 85 DEG C at this time, and stand 16 under 85 DEG C of constant temperature
~20 hours are discharged bubble thoroughly and obtain preparation liquid；
(2) it generates after step (1) is stood and without precipitating and prepares film, casting drum is heated to 100 DEG C, rotation
Roller is heated evenly by it, by step (1) preparation liquid after cylinder surface one layer of solution film of formation, standing and drying solution 10min,
Film is torn from cylinder surface,.
In the present invention, PE model 9455 used in step 3)；And the modified solution and PE of silica solution is added in graphene oxide
Dosage relation is that every 500mlPE corresponds to 0.5-1.5g graphene oxide.
The present invention selects blending and modifying solution to carry out modified poly ethylene, and selection modified material is graphene oxide@SiO2.Oxidation
The functional group of graphene can be with PE association reaction, and graphene oxide solution can prepare the solution of stable dispersion, therefore technique can
Row is good.Simultaneously because polyethylene can form a film and can pass through the modified molding that film may be implemented completely with the characteristic of glue.
Specific embodiment
The present invention is further illustrated below by embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
1 sample of table matches tables of data
| Group | Graphene oxide (g) | Silica solution (ml) | Remarks |
| 1 | 1 | 0.5 | |
| 2 | 1 | 1 | |
| 3 | 1 | 1.25 | |
| 4 | 0.5 | 1 | |
| 5 | 0.5 | 1.25 | |
| 6 | 1.5 | 0.5 | |
| 7 | 1.5 | 1 | |
| 8 | 0 | 1 | |
| 9 | 0 | 0 | PE-9455 |
According to 1 in table 1,2,3 groups of proportionate relationship prepares graphene oxide@SiO2Modified PE film, preparation process is such as
Under:
The PE of 500ml is taken to be added in beaker, water bath temperature is increased to 95 DEG C, and the beaker equipped with PE is placed in water-bath
Middle stirring makes its thawing, until above choosing no colloidal solid when being stirred for, previously configured 1,2,3 group is added at this time
Graphene oxide@SiO2Modified solution be stirred well to it and be uniformly dispersed, water temperature in water-bath is dropped to 85 DEG C at this time, is needed
Solution is stood into 16~20 hours under 85 DEG C of constant temperature, bubble in solution is discharged thoroughly, has no precipitating, obtains preparation liquid.
Casting drum is heated to 100 DEG C, pulls up heating pin later, opens favourable turn, rotation makes its roller integrally be heated
Uniformly, 5~start to operate after ten minutes.Preparation liquid is slowly poured into pallet along side, hand rest is placed below roller, level support
Rising immerses roller lower edge in solution, and roller rotation, solution forms one layer of solution film in cylinder surface, and solution is stained with to be put after a week
After standing and drying solution 10min, film is torn from cylinder surface for lower tray, with scissors by four Bian Xiuqi, a modified PE
Film.It is 1g GO0.5ml SiO with added graphene oxide quality status stamp2, 1g GO1ml SiO2With 1g GO1.25ml SiO2。
Embodiment 2
According to 4 in table 1,5 two groups of proportionate relationship prepares graphene oxide@SiO2Modified PE film, preparation process is such as
Under:
The PE of 500ml is taken to be added in beaker, water bath temperature is increased to 95 DEG C, and the beaker equipped with PE is placed in water-bath
Middle stirring makes its thawing, until above choose no colloidal solid when being stirred for, at this time plus is separately added into the 4th previously prepared
The modified solution of the 5th group of silica solution for containing 0.5g graphene oxide, is stirred well to it and is uniformly dispersed, at this time by water-bath
Middle water temperature drops to 85 DEG C, needs solution standing 16~20 hours under 85 DEG C of constant temperature, bubble in solution is discharged thoroughly, and
Without precipitating, preparation liquid is obtained.
Casting drum is heated to 100 DEG C, pulls up heating pin later, opens favourable turn, rotation makes its roller integrally be heated
Uniformly, 5~start to operate after ten minutes.Preparation liquid is slowly poured into pallet along side, hand rest is placed below roller, level support
Rising immerses roller lower edge in solution, and roller rotation, solution forms one layer of solution film in cylinder surface, and solution is stained with to be put after a week
After standing and drying solution 10min, film is torn from cylinder surface for lower tray, with scissors by four Bian Xiuqi, a modified PE
Film.It is 0.5g GO1ml SiO with added graphene oxide quality status stamp2With 0.5g GO1.25ml SiO2。
Embodiment 3
According to 6 in table 1,7 two groups of proportionate relationship prepares graphene oxide@SiO2Modified PE film, preparation process is such as
Under:
The PE of 500ml is taken to be added in beaker, water bath temperature is increased to 95 DEG C, and the beaker equipped with PE is placed in water-bath
Middle stirring makes its thawing, until above choosing no colloidal solid when being stirred for, previously the 6th 7th group of oxygen of configuration is added at this time
The modified solution of the silica gel of graphite alkene is stirred well to it and is uniformly dispersed, and water temperature in water-bath is dropped to 85 DEG C at this time, is needed
Solution is stood into 16~20 hours under 85 DEG C of constant temperature, bubble in solution is discharged thoroughly, bottom has volume precipitating to generate, and is
Prevent film forming from failing, bottom solution is abandoned, and only with top without precipitation solution, sediment fraction is the graphite oxide not being completely dissolved
Alkene, because caused by centrifugation is not thorough, so upper layer is only taken to dissolve complete solution without precipitating.
Casting drum is heated to 100 DEG C, pulls up heating pin later, opens favourable turn, rotation makes its roller integrally be heated
Uniformly, start to operate after 5~10min.Solution is slowly poured into pallet along side, hand rest is placed below roller, is held up the level of
Immerse roller lower edge in solution, roller rotation, solution forms one layer of solution film in cylinder surface, and solution is stained with to be put down after a week
After standing and drying solution 10min, film is torn from cylinder surface for pallet, with scissors by four Bian Xiuqi, a modified PE
Film.It is 1.2g GO0.5ml SiO with added graphene oxide quality status stamp2With 1.2g GO1ml SiO2。
Embodiment 4
SiO is prepared according to 8 groups of proportionate relationship in table 12Modified PE film, preparation process are as follows
The PE of 500ml is taken to be added in beaker, water bath temperature is increased to 95 DEG C, and the beaker equipped with PE is placed in water-bath
Middle stirring makes its thawing, until above choosing no colloidal solid when being stirred for, the 8th group of 1ml silicon previously prepared being added at this time
Sol solution is stirred well to it and is uniformly dispersed, and water temperature in water-bath is dropped to 85 DEG C at this time, needs solution under 85 DEG C of constant temperature
16~20 hours are stood, bubble in solution is discharged thoroughly, solution bottom has micro floccule to generate, at the bottom of when pouring into pallet
Portion's solution goes out at plume, is chosen the floccule in pallet with spoon；Illustrate the surface charge and graphene oxide particle of quantum dot
The charge on surface is electrically on the contrary, there is a natural attraction between the sexes after meeting leads to that phenomenon of flocculating occurs.And the electrical property of Particle surface charge and
How much with pH value much relations are had.The pH value of quantum dot after dilution changes, and the electrical property of surface charge is also just sent out with how many
Variation is given birth to
Casting drum is heated to 100 DEG C, pulls up heating pin later, opens favourable turn, rotation makes its roller integrally be heated
Uniformly, start to operate after 5~10min.Solution is slowly poured into pallet along side, hand rest is placed below roller, is held up the level of
Immerse roller lower edge in solution, roller rotation, solution forms one layer of solution film in cylinder surface, and solution is stained with to be put down after a week
Pallet, standing and drying solution are torn from cylinder surface after ten minutes, by film, with scissors by four Bian Xiuqi, a modified PE
Film.It is 1ml SiO with added graphene oxide quality status stamp2。
Comparative example
The PE film of Workshop Production is individually used, identical as PE model used in embodiment, property is identical.It is denoted as PE.
Experimental example:
1, the PE film provided the modified PE film of embodiment 1-4 offer, comparative example uses TU-1900/TU-1901 bis-
Light beam UV, visible light spectrophotometric photometer carries out light transmittance test.As a result as follows:
Firstly the need of the sample that film is cut into 1cm × 3cm size, it is put into laboratory apparatus by several times and is tested, final benefit
With data at figure.It is followed successively by factory's PE film, the light transmittance test of film prepared by embodiment 1,2,3,4.
It can be concluded that the PE film light transmittance that 0.5g GO is added obviously is better than other several, addition 1mlSiO2And
0.5gGO1.25mlSiO2Film light transmittance it is best, maximum value be 84.1% and 84.7%.With the increase of wavelength, film
Light transmittance be gradually increased, when wavelength is 200nm~257nm, the fluctuations of all films are maximum.It is added
1.2gGO0.5mlSiO2The film of modified solution is that 422nm~532nm has an apparent curvilinear motion in wavelength.And other 3
Kind laminated film is not much different.
It will also realize that by resulting experimental result, the PE laminated film light transmittance that graphene oxide is added is higher than the pure PE of factory
Film.And it is mixed into the PE film of 0.5g graphene oxide, that is, when concentration is 0.09%, the light transmittance of film is much higher than the pure PE of factory
Film.
2, the mechanical property that the PE film provided the modified PE film of embodiment 1-4 offer, comparative example forms a film is surveyed
Examination, it is as a result as follows.
Using standard: tensile break strength: GB1040-92 tabletting test: GB/T9053-88 ambient condition is adjusted: GB/
T2918-1982
The data of film forming are detected using high and low temperature environment electronic tension tester.Experimental sample selects same specification different
Each 3 parts of the film of material take its average value, and size of sample 100mm × 25mm is tested using the film with a thickness of 24 μm, draw
Stretching speed is 300mm/min, records the data variation in drawing process, carries out being processed into curve to data using bluehill.
Test data includes tensile strength, elongation at break and young's modulus in tension.Wherein Young's modulus is that film resists deformability
Physical quantity belongs to one kind of elasticity modulus.
Speed: 300mm/min
Note: same group every group of sample has taken three batten experiments, is average value obtained in table.
After tested, find out that the PE film stretching intensity containing 0.5gGO differs very with elongation at break with pure PE film from data
Far, it can analyze and obtain from data, it is that can increase its machinery that a certain amount of graphene oxide is added in the PE material of workshop
Intensity, as the concentration of graphene oxide is increasing, film strength is also increasing, opposes with the PVA film of sample 9
Than, it is 0.5g graphene oxide and 1ml silica solution in proportion that the modified solution of addition, which improves the elongation at break of film,
I.e. sample 4 when, the value highest of elongation at break；In terms of tensile strength, sample 2, sample 5, sample 6 improves thin with sample 8
The tensile strength of film, when proportion is 0.5g graphene oxide and 1.25ml silica solution, i.e. sample 5, the value highest of tensile strength.
From the point of view of both comprehensive, in nine groups of samples, the film that the proportion of sample 5 is produced is that tensile property is optimal.
4, the PE film provided the modified PE film of embodiment 1-4 offer, comparative example carries out surface tension test.As a result
It is as follows.
Table is each material surface tension test data
。
Claims (5)
1. a kind of graphene oxide@SiO2The method of modified poly ethylene film, which comprises the following steps:
The preparation of step 1) silica gel solution
(1) sodium metasilicate is dissolved into sodium silicate aqueous solution, the sodium silicate aqueous solution is subjected to cation exchange removal Na+, is obtained
The silicate solution for being 46% to mass fraction, wherein the partial size that cation exchanges resin used is 0.3-1.5mm, cation exchange
It is stirred in the process using paddle, mixing speed is 180-200 revs/min；
(2) to the 10% amount silicate solution for step (1) is added at 85-92 DEG C into sodium hydroxide solution obtaining, 0.8- is kept the temperature
1.2 hours obtained seed-solutions, seed-solution pH value are 9.0-9.7, and wherein the weight ratio of silicate solution and sodium hydroxide is 20:
1；
(3) seed-solution in step (2) is taken, under the conditions of temperature is 85-92 DEG C, pH value is 9.0-9.7 into the crystal seed
The silicate solution of step (1) remaining 90% amount of addition, keeps the temperature 30-45 minutes again, must synthesize dilute silica gel after charging；
(4) silicon sol solution that silica quality percentage concentration is 40% is obtained after the dilute silica gel of synthesis being concentrated by ultrafiltration；
Step 2) prepares graphene oxide modified solution
(1) graphene oxide is prepared
(2) graphene oxide prepared is added in the silica solution of step 1) preparation, it is molten obtains graphene oxide silica
Glue modified solution；It is preferred that every 0.5-1.5g graphene oxide corresponds to silica solution 0.5-1ml；
Silica gel solution modified PE film forming is added in step 3) graphene oxide:
(1) gluey PE is taken to be added in reaction vessel, temperature is increased to 95 DEG C in water-bath, and stirring makes its thawing, until again
When stirring, above choose no colloidal solid, it is modified that the graphene oxide silicon dioxide gel that step 2) prepares is added at this time
Solution is stirred well to it and is uniformly dispersed, and water temperature in water-bath is dropped to 85 DEG C at this time, and 16~20 are stood under 85 DEG C of constant temperature
A hour is discharged bubble thoroughly and obtains preparation liquid；
(2) it generates after step (1) is stood and without precipitating and prepares film, casting drum is heated to 100 DEG C, rotates roller
It is heated evenly by it, by step (1) preparation liquid after cylinder surface one layer of solution film of formation, standing and drying solution 10min, by film
It tears from cylinder surface,.
2. a kind of graphene oxide@SiO described in accordance with the claim 12The method of modified poly ethylene film, which is characterized in that oxygen
The preparation of graphite alkene the following steps are included:
A. the concentrated sulfuric acid of 60ml is added in the reaction flask that 250mL is assembled in ice-water bath, is then slowly added to 2.5g graphite powder
In the concentrated sulfuric acid, persistently stirred in ice-water bath 1 hour；
B. 10g potassium permanganate and 3.8g sodium nitrate are slowly added by several times, stirring 2 hours is continued in ice-water bath；
C. remove ice-water bath, continue to stir 2 hours at normal temperature；
D. temperature is increased to 35 DEG C, continues stirring 2 hours；
E. temperature is controlled at 98 DEG C, is slowly added to deionized water, water temperature is maintained to be kept for 1 hour at 98 DEG C, while be added and controlling
Treating percentage is that 30% hydrogen peroxide restores remaining oxidant, and mixture becomes glassy yellow from dark brown；
F. the mixture centrifuge separation obtained, and washed with 5%HCl solution and deionized water until sulfate radical-free is tested in filtrate
Until measuring；
G. filter cake is placed in 60 DEG C of vacuum oven and is sufficiently dried, saved backup.
3. a kind of graphene oxide@SiO described in accordance with the claim 12The method of modified poly ethylene film, which is characterized in that step
It is rapid 3) used in PE model 9455.
4. a kind of graphene oxide@SiO described in accordance with the claim 12The method of modified poly ethylene film, which is characterized in that oxygen
Modified solution and the PE dosage relation of silica solution is added as the corresponding 0.5-1.5g graphene oxide of every 500mlPE in graphite alkene.
5. the graphene oxide@SiO being prepared according to the described in any item sides of claim 1-42Modified poly ethylene film.
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| CN112029171A (en) * | 2020-08-21 | 2020-12-04 | 温州市中坚薄膜有限公司 | Antibacterial PE film and preparation method thereof |
| CN112358641A (en) * | 2020-11-09 | 2021-02-12 | 成都子之源绿能科技有限公司 | Heat-insulation greenhouse film and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110497633A (en) * | 2019-07-06 | 2019-11-26 | 欧名龙 | A kind of preparation method of antiultraviolet high intensity decorating film |
| CN111944189A (en) * | 2020-08-14 | 2020-11-17 | 河南师范大学 | Lignin-iron-containing PE film material and synthetic method thereof |
| CN111944189B (en) * | 2020-08-14 | 2022-05-31 | 河南师范大学 | Lignin-iron-containing PE film material and synthetic method thereof |
| CN112029171A (en) * | 2020-08-21 | 2020-12-04 | 温州市中坚薄膜有限公司 | Antibacterial PE film and preparation method thereof |
| CN112358641A (en) * | 2020-11-09 | 2021-02-12 | 成都子之源绿能科技有限公司 | Heat-insulation greenhouse film and preparation method thereof |
| CN112358641B (en) * | 2020-11-09 | 2023-01-24 | 成都子之源绿能科技有限公司 | Heat-insulation greenhouse film and preparation method thereof |
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